CN117922135B - Polyolefin waterproof coiled material and preparation and application thereof - Google Patents
Polyolefin waterproof coiled material and preparation and application thereof Download PDFInfo
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- CN117922135B CN117922135B CN202410144546.8A CN202410144546A CN117922135B CN 117922135 B CN117922135 B CN 117922135B CN 202410144546 A CN202410144546 A CN 202410144546A CN 117922135 B CN117922135 B CN 117922135B
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- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 9
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- 230000003078 antioxidant effect Effects 0.000 claims description 33
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- 239000004594 Masterbatch (MB) Substances 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
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- 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 description 1
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Landscapes
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Abstract
The invention relates to the field of polyolefin waterproof coiled materials, and discloses a polyolefin waterproof coiled material, a preparation method and an application thereof, wherein the waterproof coiled material comprises a three-layer structure, and the three-layer structure comprises a middle adhesive layer and TPO material layers arranged on the surfaces of two sides of the middle adhesive layer; the intermediate adhesive layer is formed by intermediate adhesive materials, and the composition A for forming the intermediate adhesive materials contains titanium white powder, a silane coupling agent, heavy calcium, polyisobutylene, terpene resin, C5 hydrogenated resin and butyl rubber.
Description
Technical Field
The invention relates to the field of polyolefin waterproof coiled materials, in particular to a polyolefin waterproof coiled material and preparation and application thereof.
Background
Photovoltaic grid-connected power generation application with integrated photovoltaic building as a core occupies most of the current photovoltaic market share. The photovoltaic building integration has the following advantages: the building can provide enough area for the photovoltaic system, and the building does not need to occupy additional land; the supporting structure of the photovoltaic system can be omitted, and the power transmission cost is saved; the photovoltaic array can replace conventional building materials, so that the material cost is saved; the installation is combined with the building construction, so that the installation cost is saved; the power generation is dispersed, the transmission and power distribution losses (5% -10%) are avoided, and the power transmission and power distribution investment and maintenance cost are reduced; making the appearance of the building more attractive. In addition, where power outages are often annoying, the building's photovoltaic system can become a reliable source of power.
Solar energy is combined with a building, and a house is developed into a novel building with an independent power supply and self circulation, so that the building is a necessary trend of human progress, society and scientific and technical development.
The Thermoplastic Polyolefin (TPO) waterproof coiled material mainly used for roof systems is a flaky thermoplastic rubber elastic waterproof material which is prepared by taking vinyl resin as a base material and adopting advanced polymerization technology and a specific formula, is a new material which is popular in the United states and Europe in recent years, does not contain plasticizers in ingredients, does not have the problem of embrittlement caused by plasticizer migration, and has the comprehensive characteristics of high tensile strength, good wearing resistance, strong ultraviolet resistance, smooth surface, high reflectivity, pollution resistance and the like, and is easy to process, convenient to weld and construct, and environment-friendly.
At present, H-type TPO and P-type TPO are used in roofing construction in a large amount, the construction structure is respectively a color steel tile, a vapor barrier layer, a heat insulation layer, a waterproof layer (TPO) and a protective layer (color steel tile) from bottom to top, wherein the lap joint mode of the waterproof layer can be gluing, welding and mechanical fixing, and the connection mode between the waterproof layer and the heat insulation layer and the protective layer is only one mode of mechanical fixing. In the construction of mechanical fixing method, the waterproof layer is inevitably damaged by certain penetration, and if the photovoltaic roof is mechanically fixed, the photovoltaic panel is required to be assembled and disassembled, so that the waterproof layer is more easily damaged. In order to reduce or avoid the water leakage caused by the damage, the current treatment method basically adopts a mode of repairing the damaged part, so that the procedures are increased, and the water leakage risk is increased.
CN107933034a discloses a thermoplastic polyolefin TPO waterproof coiled material, the waterproof coiled material is in a three-layer structure, the upper surface and the lower surface are both TPO coiled material layers, the middle is a polyester fiber mesh fabric reinforcing layer, wherein the TPO coiled material layer on the upper surface is white; the TPO coiled material layer is made of thermoplastic polyolefin synthetic resin material combined by ethylene propylene rubber and polypropylene as base material, modified nano calcium carbonate as filler, and anti-aging agent, tackifier, bridging agent, dispersing agent, softener and toner. However, after the waterproof coiled material is constructed, the waterproof coiled material needs to be mechanically fixed, and further repair is needed to prevent water leakage caused by the mechanical fixing part, so that the working procedures are increased, and the water leakage risk is increased.
Therefore, the development of the TPO waterproof coiled material with the self-healing function has important significance.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, in the roof construction process, when a waterproof layer and a protective layer are lapped in a mechanical fixing mode, the waterproof layer is damaged, and then a repair procedure is complicated.
In order to achieve the above object, a first aspect of the present invention provides a polyolefin waterproof roll, which contains a three-layer structure, wherein the three-layer structure is a middle adhesive layer and TPO material layers disposed on two side surfaces of the middle adhesive layer;
The intermediate adhesive layer is formed by an intermediate adhesive material, and the composition A forming the intermediate adhesive material contains titanium white powder, a silane coupling agent, heavy calcium I, polyisobutene, terpene resin, C5 hydrogenated resin and butyl rubber;
the content of the titanium pigment is 6-10 parts by weight, the content of the silane coupling agent is 0.5-2 parts by weight, the content of the heavy calcium I is 85-110 parts by weight, the content of the polyisobutene is 75-95 parts by weight, the content of the terpene resin is 35-50 parts by weight, and the content of the C5 hydrogenated resin is 70-85 parts by weight relative to 100 parts by weight of the butyl rubber;
In the composition A, the polymerization degree of the polyisobutene is 1000-1400; the softening point of the terpene resin is 80-125 ℃, and the kinematic viscosity at 190 ℃ is 100-300 mPa.s; the softening point of the C5 hydrogenated resin is 90-150 ℃, and the kinematic viscosity at 200 ℃ is 100-400 mPa.s.
The second aspect of the present invention provides a method for preparing a polyolefin waterproof roll, the method comprising:
(1) Preparing a sizing material for the intermediate glue layer: mixing and contacting the components in the composition A for forming the intermediate adhesive material in the first aspect to obtain the adhesive material for the intermediate adhesive layer;
And
Forming a TPO material layer I by using the main waterproof material;
(2) Coating the intermediate adhesive layer on the TPO material layer I to form an intermediate body containing the intermediate adhesive layer;
(3) And forming a TPO material layer II by applying a main waterproof material on the intermediate adhesive layer of the intermediate to obtain the polyolefin waterproof coiled material containing the TPO material layer II.
A third aspect of the present invention provides a polyolefin waterproof roll obtained by the production method described in the foregoing second aspect.
A fourth aspect of the present invention provides the use of the polyolefin waterproof roll described in the foregoing third aspect in the waterproof field of buildings.
Through the technical scheme, the invention has at least the following advantages:
(1) The polyolefin waterproof coiled material provided by the invention can be directly paved in application construction, only the long side and the short side of the coiled material are required to be welded, and the short side can be glued.
(2) Compared with the conventional H-type TPO, the TPO with the self-adhesive layer and the conventional P-type TPO, the polyolefin waterproof coiled material provided by the invention has better waterproof effect, and the intermediate adhesive layer has very good creep property and self-healing property, and in the construction of a mechanical fixing method, the polyolefin waterproof coiled material can automatically repair the penetrating damage part, so that the construction process is simpler, and the procedures of subsequent reprocessing of mechanical fixing after the coiled material is paved are reduced.
(3) The polyolefin waterproof coiled material provided by the invention has multiple layers of materials with different heat conductivity coefficients, so that heat conduction is more difficult, wherein the heat conductivity coefficient of the middle adhesive layer is low, the heat conduction is slow, and a certain heat preservation effect can be achieved.
(4) The polyolefin waterproof coiled material provided by the invention has better heat aging performance, weather resistance and chemical corrosion resistance, and corresponding accelerated aging and chemical corrosion tests are carried out in an experimental environment.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As described above, the first aspect of the present invention provides a polyolefin waterproof roll, which contains a three-layer structure, wherein the three-layer structure is a middle adhesive layer and TPO material layers disposed on two side surfaces of the middle adhesive layer;
The intermediate adhesive layer is formed by an intermediate adhesive material, and the composition A forming the intermediate adhesive material contains titanium white powder, a silane coupling agent, heavy calcium I, polyisobutene, terpene resin, C5 hydrogenated resin and butyl rubber;
the content of the titanium pigment is 6-10 parts by weight, the content of the silane coupling agent is 0.5-2 parts by weight, the content of the heavy calcium I is 85-110 parts by weight, the content of the polyisobutene is 75-95 parts by weight, the content of the terpene resin is 35-50 parts by weight, and the content of the C5 hydrogenated resin is 70-85 parts by weight relative to 100 parts by weight of the butyl rubber;
In the composition A, the polymerization degree of the polyisobutene is 1000-1400; the softening point of the terpene resin is 80-125 ℃, and the kinematic viscosity at 190 ℃ is 100-300 mPa.s; the softening point of the C5 hydrogenated resin is 90-150 ℃, and the kinematic viscosity at 200 ℃ is 100-400 mPa.s.
Preferably, in the composition A, the mean particle size of the heavy calcium I is from 2 to 30. Mu.m.
Preferably, in the composition a, the terpene resin is an α -terpene resin.
Preferably, in the composition A, the density of the butyl rubber is 0.8-1.5g/cm3.
Preferably, in the composition A, the titanium pigment has an average particle diameter of 0.1-10 μm.
According to a preferred embodiment, the intermediate gum material-forming composition a also contains an anti-uv agent I and an antioxidant; the content of the ultraviolet resistance agent I is 0.75-1.5 parts by weight and the content of the antioxidant is 1.5-4 parts by weight relative to 100 parts by weight of the butyl rubber. The inventors of the present invention found that, in this preferred case, the polyolefin waterproof roll provided by the present invention is higher in heat aging property.
More preferably, in the composition a, the antioxidant is in a content mass ratio of 1:0.8-1.2 of antioxidant 168 and antioxidant 1010.
According to a preferred embodiment, the two TPO material layers are formed by a main waterproof material, and the composition B for forming the main waterproof material contains polypropylene, heavy calcium II, polyolefin elastomer I, composite antioxidant master batch and color master batch; based on the total weight of the composition B, the content of the polypropylene is 25-35wt%, the content of the heavy calcium II is 15-20wt%, the content of the polyolefin elastomer I is 40-50wt%, the content of the composite antioxidant master batch is 3-5wt%, and the content of the color master batch is 2-4wt%.
Preferably, in said composition B, the polypropylene has a melt index of 2-5g/10min and a density of 0.7-1.2g/cm 3 at 230℃and 2.16 Kg.
Preferably, in said composition B, said polyolefin elastomer I has a melt index of 1.0 to 8.0g/10min and a density of 0.6 to 1.2g/cm 3 at 230℃and 2.16 Kg.
Preferably, in the composition B, the mean particle size of the heavy calcium II is 1-20 μm.
Preferably, in the composition B, the average particle size of the color master is 1 to 6mm.
Preferably, in the composition B, the composite antioxidant masterbatch is prepared by mixing the following components in mass ratio of 7:0.8-1.2:0.8-1.2: and 0.8-1.2 of polyolefin elastomer II, an antioxidant, an ultraviolet resistant agent II and a light stabilizer.
Preferably, the conditions of the mixing reaction include: the temperature is 160-190 ℃ and the time is 5-30min.
In order to obtain a polyolefin waterproof roll with better heat aging performance, it is preferable that the polyolefin elastomer I and the polyolefin elastomer II are the same substance.
In the polyolefin waterproof roll, the main waterproof materials of the two TPO material layers may be the same or different, and the composition B forming the main waterproof materials may be the same or different.
In order to obtain a polyolefin waterproof roll with better heat insulation performance, according to a preferred embodiment, the color master of the composition B of the main material of the TPO material layer is optionally white master.
In order to obtain a polyolefin waterproof roll with better heat insulation performance, according to another preferred embodiment, the color masterbatch in the composition B of the main proofing material of one of the TPO material layers is selected to be 1:1.5-2.5 of black and white.
As described above, the second aspect of the present invention provides a method for preparing a polyolefin waterproof roll, the method comprising:
(1) Preparing a sizing material for the intermediate glue layer: mixing and contacting the components in the composition A for forming the intermediate adhesive material in the first aspect to obtain the adhesive material for the intermediate adhesive layer;
And
Forming a TPO material layer I by using the main waterproof material;
(2) Coating the intermediate adhesive layer on the TPO material layer I to form an intermediate body containing the intermediate adhesive layer;
(3) And forming a TPO material layer II by applying a main waterproof material on the intermediate adhesive layer of the intermediate to obtain the polyolefin waterproof coiled material containing the TPO material layer II.
The specific method for the mixed contact in the step (1) of preparing the intermediate gum layer rubber compound is not particularly limited, and may be performed by methods known in the art, and, for example, titanium white powder, a silane coupling agent, heavy calcium I, polyisobutylene, a terpene resin, a C5 hydrogenated resin and butyl rubber may be mixed contacted. However, in order to obtain a polyolefin waterproof roll having higher self-healing properties, the present invention preferably employs the preferred embodiments described below for the mixed contact.
According to a particularly preferred embodiment, in step (1), the operation of mixing contact comprises:
(a1) The method comprises the steps of (1) carrying out first stirring and mixing on a material I containing titanium dioxide, an ultraviolet resistant agent I, an antioxidant, heavy calcium I, polyisobutylene, terpene resin, C5 hydrogenated resin and butyl rubber to obtain a mixture I;
(a2) And (3) carrying out second stirring and mixing on the mixture I and the silane coupling agent to obtain the sizing material for the intermediate glue layer.
Preferably, in the composition A, the titanium pigment is used in an amount of 6 to 10 parts by weight, the silane coupling agent is used in an amount of 0.5 to 2 parts by weight, the heavy calcium I is used in an amount of 85 to 110 parts by weight, the polyisobutylene is used in an amount of 75 to 95 parts by weight, the terpene resin is used in an amount of 35 to 50 parts by weight, and the C5 hydrogenated resin is used in an amount of 70 to 85 parts by weight, relative to 100 parts by weight of the butyl rubber; the dosage of the ultraviolet resistance agent I is 0.75-1.5 weight parts, and the dosage of the antioxidant is 1.5-4 weight parts.
Preferably, in step (a 1), the first stirring and mixing conditions include: the temperature is 120-140 ℃ and the time is 2-4h.
Preferably, in step (a 2), the second stirring and mixing conditions include: the temperature is 120-140 ℃ and the time is 0.5-1h.
In order to obtain a polyolefin waterproofing membrane with better self-healing properties, according to another particularly preferred embodiment, the operation of mixed contact comprises:
(S1) carrying out first stirring on the preheated and melted butyl rubber, titanium white powder, an ultraviolet resistant agent I, an antioxidant, C5 hydrogenated resin, terpene resin and a first part of heavy calcium I to obtain a stirring mixture I;
(S2) carrying out second stirring on the stirring mixture I, the first part of polyisobutene and the second part of heavy calcium I to obtain a stirring mixture II;
and (S3) carrying out third stirring on the stirring mixture II, the rest polyisobutylene, the rest heavy calcium I and the silane coupling agent to obtain the sizing material for the intermediate glue layer.
In the operation of the mixed contact, the heavy calcium I can be added in one step or in multiple steps, and particularly preferably, the heavy calcium I is added in three steps, wherein the amount of the heavy calcium I in the first part is 40-60wt% of the total amount of the heavy calcium I, the amount of the heavy calcium I in the second part is 20-30wt% of the total amount of the heavy calcium I, and the amount of the residual heavy calcium I is 20-30wt% of the total amount of the heavy calcium I. The sum of the amount of the first part of heavy calcium I, the amount of the second part of heavy calcium I and the amount of the remaining heavy calcium I is equal to the total amount of heavy calcium I in the first aspect. The inventor of the present invention found that in this preferred case, the polyolefin waterproof roll provided by the present invention has better self-healing properties.
In the operation of the mixing contact, the polyisobutene may be added in one portion or in two portions, particularly preferably in two portions, the amount of the first portion being from 40 to 60% by weight of the total amount of the polyisobutene and the amount of the remainder being from 40 to 60% by weight of the total amount of the polyisobutene. The sum of the amount of the first portion of polyisobutene and the amount of the polyisobutene remaining is equal to the total amount of polyisobutene in the first aspect. The inventor of the present invention found that in this preferred case, the polyolefin waterproof roll provided by the present invention has better self-healing properties.
Preferably, in step (S1), the preheating and melting operations include: preheating the butyl rubber at 120-140 ℃ for 0.5-1.5h.
Preferably, in step (S1), the first stirring condition includes: the temperature is 120-140 ℃ and the time is 0.5-1h.
Preferably, in step (S2), the second stirring condition includes: the temperature is 120-140 deg.C, and the time is 15-45min.
Preferably, in step (S3), the third stirring condition includes: the temperature is 120-140 ℃ and the time is 1-1.5h.
Preferably, in step (1), the preparation method further comprises preparing the main waterproof material by using a step comprising: the components of the composition B for forming a main waterproof material in the first aspect are melt-blended to obtain the main waterproof material.
Preferably, the conditions of melt blending include: the barrel temperature is 170-190 ℃, the temperature of the three-roller calender is 45-65 ℃, and the temperature of the tempering roller is 30-45 ℃.
Preferably, the conditions of melt blending further comprise: the time is 1-10h.
Preferably, in the composition B, the polypropylene is used in an amount of 25 to 35wt%, the heavy calcium II is used in an amount of 15 to 20wt%, the polyolefin elastomer I is used in an amount of 40 to 50wt%, the composite antioxidant masterbatch is used in an amount of 3 to 5wt%, and the masterbatch is used in an amount of 2 to 4wt%, based on the total weight of the composition B.
In step (1), the operation of forming the TPO material layer I using the main waterproof material may be performed by a conventional operation in the art, and, for example, the TPO material layer I may be formed by extrusion or the TPO material layer II may be formed.
It should be noted that, in the present invention, all stirring rates involved in the stirring step are not particularly limited, and may be carried out at stirring rates conventional in the art.
In the step (2), the intermediate adhesive layer may be melted with a sizing material and then coated on the TPO material layer I to form an intermediate including the intermediate adhesive layer. The conditions of the melting are not particularly limited in the present invention, and the conventional operation in the art may be employed.
Preferably, in the step (3), after the main waterproof material is first applied to form the TPO material layer II, the intermediate adhesive layer of the intermediate and the TPO material layer II are bonded to obtain the polyolefin waterproof roll containing the TPO material layer II.
Preferably, in the step (3), the intermediate polyethylene waterproof roll is subjected to welding treatment at any side length, so that the polyolefin waterproof roll with better self-healing property and waterproof performance can be obtained. The welding process may be performed using methods conventional in the art.
As described above, the third aspect of the present invention provides a polyolefin waterproof roll obtained by the production method described in the second aspect.
Preferably, the thickness of the TPO material layer I is 0.5-0.9mm, the thickness of the TPO material layer II is 0.5-0.9mm, and the thickness of the intermediate adhesive layer is 0.3-0.35mm.
As described above, a fourth aspect of the present invention provides the use of the polyolefin waterproof roll described in the foregoing third aspect in the waterproof field of construction.
The invention will be described in detail below by way of examples. In the following examples, unless otherwise specified, various materials and instruments were used as commercial products, and specific sources of the materials are shown in Table 1.
TABLE 1
The A series preparation example of the invention is used for preparing the composite antioxidant master batch.
Preparation example A1
70G of polyolefin elastomer II, 10g of antioxidant, 10g of ultraviolet resistance agent II and 10g of light stabilizer are mixed to react to prepare the composite antioxidant master batch which is named M-1.
Unless otherwise specified, the A-series preparation was carried out by referring to the method of preparation A1, except that the amounts of raw materials and the process parameters used in the remaining A-series preparations were different, specifically referring to Table 2.
TABLE 2
| Raw material name | Preparation example A1 | Preparation example A2 | Preparation example A3 |
| Polyolefin elastomer II/g | 70 | 70 | 70 |
| Antioxidant/g | 10 | 9 | 7 |
| Uvioresistant agent II/g | 10 | 9 | 10 |
| Light stabilizers/g | 10 | 12 | 13 |
| Mixing reaction | |||
| Time/min | 30 | 10 | 6 |
| Temperature/. Degree.C | 160 | 180 | 190 |
| Naming the name | M-1 | M-2 | M-3 |
The preparation examples of the B series of the invention are used for preparing the sizing material for the intermediate glue layer.
The amounts of the raw materials used in the preparation examples of the B series are parts by weight, unless otherwise specified, and each part by weight represents 1g.
Preparation example B1
(S1) carrying out first stirring on the preheated and melted butyl rubber, titanium white powder, an ultraviolet resistant agent I, an antioxidant, C5 hydrogenated resin, terpene resin and a first part of heavy calcium I to obtain a stirring mixture I;
(S2) carrying out second stirring on the stirring mixture I, the first part of polyisobutene and the second part of heavy calcium I to obtain a stirring mixture II;
(S3) stirring the stirring mixture II, the residual polyisobutene, the residual heavy calcium I and the silane coupling agent for the third time to obtain the sizing material J-1 for the intermediate glue layer.
The first part of heavy calcium I is 50wt% of the total heavy calcium I, the second part of heavy calcium I is 25wt% of the total heavy calcium I, and the rest of heavy calcium I is 25wt% of the total heavy calcium I.
The amount of the first portion of polyisobutene was 50% by weight based on the total amount of polyisobutene, the remainder of the polyisobutene being 50% by weight based on the total amount of polyisobutene.
Preparation example B2
The preparation example was conducted by referring to the method of preparation example B1, except that the raw materials and the process parameters used in the preparation example were different, and a rubber compound J-2 for an intermediate rubber layer was obtained. The specific amounts of the raw materials are shown in Table 3, and the specific process parameters are shown in Table 4.
The first part of heavy calcium I is 42wt% of the total heavy calcium I, the second part of heavy calcium I is 28wt% of the total heavy calcium I, and the rest of heavy calcium I is 30wt% of the total heavy calcium I.
The amount of the first portion of polyisobutene was 42% by weight based on the total amount of polyisobutene, the remainder of the polyisobutene being 58% by weight based on the total amount of polyisobutene.
Preparation example B3
The preparation example was conducted by referring to the method of preparation example B1, except that the raw materials and the process parameters used in the preparation example were different, and a rubber compound J-3 for an intermediate rubber layer was obtained. The specific amounts of the raw materials are shown in Table 3, and the specific process parameters are shown in Table 4.
In this preparation, the amounts of the heavy calcium I and the polyisobutene added in portions were the same as in preparation B1.
Preparation example B4
This preparation was conducted by referring to the method of preparation B1 except that the same weight parts of terpene resin II was used in place of terpene resin I in preparation B1 to give size J-4 for an intermediate layer.
Comparative preparation D-B1
This comparative preparation was carried out with reference to the process of preparation B1, except that the polyisobutene I of preparation B1 was replaced with an equal part by weight of polyisobutene II, giving a size D-J1 for the intermediate layer.
The addition amounts of the heavy calcium I and the polyisobutene in the comparative preparation example are the same as those of the preparation example B1.
Preparation example D-B2
This comparative preparation was conducted by referring to the method of preparation B1 except that the amount of the hydrogenated C5 resin I used in this comparative preparation was adjusted to 87 parts by weight, to obtain a rubber D-J2 for an intermediate layer.
Preparation example D-B3
This comparative preparation was conducted by referring to the method of preparation B1 except that the same weight part of C5 hydrogenated resin III was used in place of C5 hydrogenated resin I in preparation B1 to obtain rubber D-J3 for the intermediate layer.
Preparation example D-B4
This comparative preparation was conducted by referring to the method of preparation B1 except that no terpene resin was added in this comparative preparation to obtain a compound D-J4 for an intermediate layer.
TABLE 3 Table 3
| Raw material name | Preparation example B1 | Preparation example B2 | Preparation example B3 |
| Butyl rubber/parts by weight | 100 | 100 | 100 |
| Titanium pigment per weight portion | 8.3 | 7.1 | 9.5 |
| Silane coupling agent per weight part | 0.8 | 1.2 | 1.8 |
| Heavy calcium/weight part | 97.9 | 105 | 90 |
| Polyisobutene (S) | |||
| Species of type | Polyisobutene I | Polyisobutene I | Polyisobutene I |
| Parts by weight of | 85 | 90 | 80 |
| Terpene resin | |||
| Species of type | Terpene resin I | Terpene resin I | Terpene resin I |
| Parts by weight of | 41.7 | 38.2 | 48.5 |
| C5 hydrogenated resin | |||
| Species of type | C5 hydrogenated resin I | C5 hydrogenated resin I | C5 hydrogenated resin II |
| Parts by weight of | 79.2 | 82 | 70 |
| Ultraviolet resistance agent I | 1.3 | 0.81 | 1.5 |
| Antioxidant agent | |||
| Species of type | Antioxidant I | Antioxidant I | Antioxidant I |
| Parts by weight of | 1.3 | 1.2 | 1.5 |
| Species of type | Antioxidant II | Antioxidant II | Antioxidant II |
| Parts by weight of | 1.3 | 1.3 | 1.2 |
TABLE 4 Table 4
| Process steps | Preparation example B1 | Preparation example B2 | Preparation example B3 |
| Preheating and melting | |||
| Temperature/. Degree.C | 130 | 135 | 120 |
| Time/h | 1 | 0.8 | 1.5 |
| First stirring | |||
| Temperature/. Degree.C | 120 | 135 | 135 |
| Time/h | 1 | 0.8 | 0.8 |
| Second stirring | |||
| Temperature/. Degree.C | 130 | 140 | 120 |
| Time/min | 30 | 15 | 45 |
| Third stirring | |||
| Temperature/. Degree.C | 130 | 140 | 120 |
| Time/h | 1.2 | 1 | 1.5 |
The C series preparation examples of the present invention are used for preparing TPO material layers, and the total amount of the composition B in the C series preparation examples is 1Kg.
Preparation C1
And (3) melting and blending the polypropylene, the heavy calcium II, the polyolefin elastomer I, the composite antioxidant master batch and the color master batch to obtain a main waterproof material, and extruding to obtain the TPO material layer. The specific amounts of the raw materials and the process parameters are shown in Table 5.
The rest of the C series preparation examples were carried out by referring to the method of preparation example C1, except that the types, amounts of raw materials and process parameters of preparation were different, and are specifically shown in Table 5.
TABLE 5
| Raw material name | Preparation C1 | PREPARATION EXAMPLE C2 | PREPARATION EXAMPLE C3 |
| Polypropylene | |||
| Species of type | Polypropylene I | Polypropylene I | Polypropylene I |
| Amount/wt% | 30 | 30 | 28 |
| Heavy calcium II/wt% | 18 | 18 | 15 |
| Polyolefin elastomer I/wt% | 45 | 45 | 49 |
| Composite antioxidant master batch | |||
| Species of type | M-1 | M-1 | M-2 |
| Amount/wt% | 4 | 4 | 4 |
| Color masterbatch | |||
| Species of type | Color masterbatch II | Color masterbatch II | Color masterbatch II |
| Amount/wt% | 3 | 2 | 4 |
| Species of type | / | Color masterbatch I | |
| Amount/wt% | / | 1 | |
| Melt blending | |||
| Barrel temperature/. Degree.C | 180 | 180 | 180 |
| Temperature/. Degree.C. of three-roll calender | 50 | 50 | 50 |
| Tempering roll temperature/°c | 40 | 40 | 40 |
| Time/h | 5 | 5 | 8 |
| Naming the name | T-1 | T-2 | T-3 |
| Thickness/mm | 0.8 | 0.5 | 0.7 |
PREPARATION EXAMPLE C4
Preparation example C4 was conducted by referring to the method of preparation example C1, except that in preparation example C4, the composite antioxidant master batch M-1 in preparation example C1 was replaced with the composite antioxidant master batch M-3 of equal mass to obtain a TPO material layer T-4.
PREPARATION EXAMPLE C5
Preparation example C5 was conducted by referring to the method of preparation example C1, except that in preparation example C5, polypropylene I in preparation example C1 was replaced with polypropylene II of equal quality to obtain TPO material layer T-5.
Examples
(1) Coating a sizing material for an intermediate glue layer on the TPO material layer I to form an intermediate containing the intermediate glue layer;
(2) And bonding a TPO material layer II on the intermediate adhesive layer of the intermediate to obtain the polyolefin waterproof coiled material containing the TPO material layer II.
The sizing materials for the TPO material layer and the intermediate adhesive layer used for preparing the polyolefin waterproof coiled material are shown in Table 6.
TABLE 6
Test case
The polyolefin waterproof coiled material prepared in the example is subjected to TPO material layer mechanics, waterproof and middle glue layer performance test, and the main test standard is GB27789-2011/GBT23260-2009. The specific test results are shown in Table 7.
The method for testing the pullout strength comprises the following steps: the polyolefin waterproof coiled material is penetrated by a carbon steel screw with the diameter of 6.3mm, and after the polyolefin waterproof coiled material is placed for 48 hours in a standard test environment, the nail pulling force value is tested.
Water impermeability after nailing: the polyolefin waterproof coiled material is penetrated by a carbon steel screw with the diameter of 6.3mm, and after the polyolefin waterproof coiled material is placed for 48 hours in a standard test environment, the water impermeability of the nailing part is tested.
TABLE 7
Continuous table 7
As can be seen from the results in Table 7, the polyolefin waterproof coiled material provided by the invention has good mechanical properties, excellent ageing resistance, weather resistance and chemical resistance, better self-healing property, stronger pulling strength and the like.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (11)
1. The polyolefin waterproof coiled material is characterized by comprising a three-layer structure, wherein the three-layer structure comprises a middle adhesive layer and TPO material layers arranged on the two side surfaces of the middle adhesive layer;
The intermediate adhesive layer is formed by an intermediate adhesive material, and the composition A forming the intermediate adhesive material contains titanium white powder, a silane coupling agent, heavy calcium I, polyisobutene, terpene resin, C5 hydrogenated resin and butyl rubber;
the content of the titanium pigment is 6-10 parts by weight, the content of the silane coupling agent is 0.5-2 parts by weight, the content of the heavy calcium I is 85-110 parts by weight, the content of the polyisobutene is 75-95 parts by weight, the content of the terpene resin is 35-50 parts by weight, and the content of the C5 hydrogenated resin is 70-85 parts by weight relative to 100 parts by weight of the butyl rubber;
In the composition A, the polymerization degree of the polyisobutene is 1000-1400; the softening point of the terpene resin is 80-125 ℃, and the kinematic viscosity at 190 ℃ is 100-300 mPa.s; the softening point of the C5 hydrogenated resin is 90-150 ℃, and the kinematic viscosity at 200 ℃ is 100-400 mPa.s;
The TPO material layers on the two side surfaces are formed by main waterproof materials, and a composition B for forming the main waterproof materials contains polypropylene, heavy calcium II, polyolefin elastomer I, composite antioxidant master batch and color master batch;
Based on the total weight of the composition B, the content of the polypropylene is 25-35wt%, the content of the heavy calcium II is 15-20wt%, the content of the polyolefin elastomer I is 40-50wt%, the content of the composite antioxidant master batch is 3-5wt%, and the content of the color master batch is 2-4wt%.
2. The polyolefin waterproof roll according to claim 1, wherein in the composition a, the average particle diameter of the heavy calcium I is 2 to 30 μm;
And/or, in the composition a, the terpene resin is an α -terpene resin.
3. The polyolefin waterproof roll according to claim 1 or2, wherein the intermediate gum material forming composition a further comprises an anti-uv agent I and an antioxidant;
The content of the ultraviolet resistance agent I is 0.75-1.5 parts by weight and the content of the antioxidant is 1.5-4 parts by weight relative to 100 parts by weight of the butyl rubber.
4. The polyolefin waterproof roll according to claim 1 or 2, wherein in the composition B, the polypropylene has a melt index of 2 to 5g/10min at 230 ℃ under 2.16Kg and a density of 0.7 to 1.2g/cm 3;
And/or in the composition B, the polyolefin elastomer I has a melt index of 1.0-8.0g/10min and a density of 0.6-1.2g/cm 3 at 230 ℃ and 2.16 Kg;
And/or, in the composition B, the heavy calcium II has an average particle size of 1-20 μm;
And/or in the composition B, the composite antioxidant masterbatch is prepared from the following components in percentage by mass: 0.8-1.2:0.8-1.2: and 0.8-1.2 of polyolefin elastomer II, an antioxidant, an ultraviolet resistant agent II and a light stabilizer.
5. A method for producing the polyolefin waterproof roll as claimed in any one of claims 1 to 4, characterized in that the method comprises:
(1) Preparing a sizing material for the intermediate glue layer: mixing and contacting all components in the composition A for forming the intermediate adhesive material to obtain the adhesive material for the intermediate adhesive layer;
And
Forming a TPO material layer I by using the main waterproof material;
(2) Coating the intermediate adhesive layer on the TPO material layer I to form an intermediate body containing the intermediate adhesive layer;
(3) And forming a TPO material layer II by applying a main waterproof material on the intermediate adhesive layer of the intermediate to obtain the polyolefin waterproof coiled material containing the TPO material layer II.
6. The method of claim 5, wherein in step (1), the operation of mixing and contacting comprises:
(a1) The method comprises the steps of (1) carrying out first stirring and mixing on a material I containing titanium dioxide, an ultraviolet resistant agent I, an antioxidant, heavy calcium I, polyisobutylene, terpene resin, C5 hydrogenated resin and butyl rubber to obtain a mixture I;
(a2) And (3) carrying out second stirring and mixing on the mixture I and the silane coupling agent to obtain the sizing material for the intermediate glue layer.
7. The method of claim 6, wherein in step (a 1), the first agitation mixing conditions include: the temperature is 120-140 ℃ and the time is 2-4h;
And/or, in step (a 2), the second agitation mixing conditions include: the temperature is 120-140 ℃ and the time is 0.5-1h.
8. The production method according to claim 6 or 7, characterized in that in step (1), the production method further comprises producing the main waterproof material by a step comprising:
the components of composition B for forming the primary waterproof material are melt blended to obtain the primary waterproof material.
9. The method of preparing according to claim 8, wherein the conditions of melt blending comprise: the barrel temperature is 170-190 ℃, the temperature of the three-roller calender is 45-65 ℃, and the temperature of the tempering roller is 30-45 ℃.
10. A polyolefin waterproof roll obtained by the production process according to any one of claims 5 to 9.
11. Use of the polyolefin waterproofing membrane of claim 10 in the field of waterproofing of buildings.
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| CN107722474A (en) * | 2017-09-08 | 2018-02-23 | 张家港爱科思汽车配件有限公司 | A kind of butyl damping material |
| CN107933034A (en) * | 2017-11-21 | 2018-04-20 | 广西武宣金牌防水材料科技有限公司 | Thermoplastic polyolefin TPO waterproof rolls and preparation method thereof |
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| WO2021189584A1 (en) * | 2020-03-27 | 2021-09-30 | 山东双圆密封科技有限公司 | Exposed weather-resistant aluminium foil heat-insulated self-adhesive waterproofing coiled material and preparation method therefor |
| CN117070166B (en) * | 2023-08-08 | 2024-04-02 | 德州科顺建筑材料有限公司 | Adhesive layer composition, polyolefin waterproof coiled material, and preparation method and application thereof |
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| CN107722474A (en) * | 2017-09-08 | 2018-02-23 | 张家港爱科思汽车配件有限公司 | A kind of butyl damping material |
| CN107933034A (en) * | 2017-11-21 | 2018-04-20 | 广西武宣金牌防水材料科技有限公司 | Thermoplastic polyolefin TPO waterproof rolls and preparation method thereof |
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