CN110408340A - A kind of reaction bonded wet-laying polymer membranes and preparation method thereof - Google Patents
A kind of reaction bonded wet-laying polymer membranes and preparation method thereof Download PDFInfo
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- CN110408340A CN110408340A CN201910706235.5A CN201910706235A CN110408340A CN 110408340 A CN110408340 A CN 110408340A CN 201910706235 A CN201910706235 A CN 201910706235A CN 110408340 A CN110408340 A CN 110408340A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J195/00—Adhesives based on bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/241—Polyolefin, e.g.rubber
- C09J7/243—Ethylene or propylene polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D31/00—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution
- E02D31/02—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution against ground humidity or ground water
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/66—Sealings
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
- E04D5/00—Roof covering by making use of flexible material, e.g. supplied in roll form
- E04D5/10—Roof covering by making use of flexible material, e.g. supplied in roll form by making use of compounded or laminated materials, e.g. metal foils or plastic films coated with bitumen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
- C09J2423/046—Presence of homo or copolymers of ethene in the substrate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2495/00—Presence of bitume
Abstract
The present invention provides a kind of reaction bonded wet-laying polymer membranes and preparation method thereof, belongs to waterproof material technical field.The waterproof roll includes the polyolefin thermoplastic elastomer base for being located at upper layer, is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, and polyolefin thermoplastic elastomer is mainly prepared from the following raw materials: polyisobutene, the copolymer of ethylene and octene, EP rubbers, modified polypropene, antioxidant, age resister, softening agent, filler material；Preparation method be after preparing modified pitch binder and polyolefin thermoplastic elastomer respectively by the two thermo-compression bonding, control thick sizing, and cover isolation film protective layer, winding is made.The waterproof roll is by making the tire base that performance is more adapted to modified pitch binder, by increasing the cracking resistance of tire base and increasing cohesive force between modified pitch binder and tire base, it avoids coiled material from crack occur, ensure that the waterproof sealing effect of coiled material.
Description
[technical field]
The present invention relates to waterproof roll technical fields, and in particular to a kind of reaction bonded wet-laying polymer membranes and its
Preparation method.
[background technique]
Waterproof roll is mainly used for construction wall, roofing and tunnel, highway, subway, refuse landfill etc., rises
To the rollable flexible building material product at web-like of one kind for resisting extraneous rainwater, underground water leakage, as engineering foundation and building
Ne-leakage connects between object, is the first barrier of entire engineering waterproofing, plays a crucial role to entire engineering, according to
Its main waterproof composition material can be divided into asphalt waterproofing material, modified-high polymer waterproof roll material and synthetic polymeric waterproofing material three
Major class.Asphalt water-proof coiled material asphalt water-proof coiled material is after invading pitching on base tire (such as body paper, fabric), then spreads on surface
Cloth powdery or the isolated material of sheet and manufactured rollable sheet waterproof material, therefore, traditional asphalt waterproof material use the longevity
Short, poor chemical stability is ordered, and waterproof effect is undesirable.With going out for the macromolecular sheet material of asphalt water-proof coiled material or fabric layer
It is existing, because it can be easy to use with industrialized production, using increasingly having been favored by people in construction, especially
The construction of building top layer terrace, subway terrace and dykes and dams culverts and water gates top surface, the one side by modified bituminous pitch coiled material with adhesive are direct
It pastes concrete surface and just achievees the purpose that waterproof.
Currently, the waterproof roll that waterproof effect is ideal, be generated by pitch and crosslinking agent mixing chemical crosslinking and
Physics mortise and tenon acts on enhancing the cementation power of waterproof roll and concrete surface, promotes the effect of waterproof, and can be in humidity
Paving is carried out on basal plane, increases the convenience of construction.But current reaction bonded wet-laying polymer membranes is using
The case where having following defects that if paved surface generates crack in, coiled material caused to stretch, as stretching cannot be alleviated in the base of coiled material
When the tensile stress that is formed, be easy to cause coiled material crack occur and be even broken, influence the sealing performance of coiled material.
[summary of the invention]
Goal of the invention of the invention is: in view of the above problems, it is anti-to provide a kind of reaction bonded wet-laying macromolecule
Water coiled material and preparation method thereof, the waterproof roll are led to by making the tire base that performance is more adapted to modified pitch binder
It crosses the cracking resistance for increasing tire base and increases cohesive force between modified pitch binder and tire base, coiled material is avoided to split
Seam, ensure that the waterproof sealing effect of coiled material.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of reaction bonded wet-laying polymer membranes, including be located at upper layer polyolefin thermoplastic elastomer base,
It is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, specifically:
The adhesive layer is mainly made of raw material from the following weight: 55~60 parts of asphalt, tackifier 7~10
Part, 5~10 parts of plasticizer, 0.5~1 part of antioxidant, 0.5~2 part of crosslinking agent, 0.2~0.6 part of crosslinking accelerator, filler material
20~30 parts；
The polyolefin thermoplastic elastomer is mainly made of raw material from the following weight: molecular weight is 10,000~100,
20~30 parts of copolymer, the EP rubbers 3 of 000 5~10 parts of polyisobutene, the ethylene that molecular weight is 1000~3500 and octene
~6 parts, 10~25 parts of modified polypropene, 1.2~2.0 parts of antioxidant, 1.0~2.0 parts of age resister, 1~3 part of softening agent, fill out
20~30 parts of charge；Wherein, the filler material be precipitated calcium carbonate that mass ratio is 1-3:6 and bentonite it is mixed and modified after it is mixed
Close object.
Further, the modified polypropene is to be prepared by the following method and obtain: average molecular weight of making even be 50,000~
300,000 50~70 parts of polypropylene, 20~30 parts of chlorinated polypropylene, 3~5 parts of zinc naphthenate catalyst, 120 DEG C~210
It is stirred to react 20~40min at a temperature of DEG C, is then granulated into particulate matter.
Further, the modified alta-mud is prepared by the following method to obtain: taking precipitated calcium carbonate and swollen by weight
Profit earth mixtures dehydrates under conditions of 110~120 DEG C, is then added in high-speed mixer, in 75~90 DEG C of condition
Lower that modifying agent is added into mixture, modified 10~15min, obtains filler material under the high-speed stirred of 1000-1300r/min；
Wherein the dosage of modifying agent is the 2.5-3.0% of the precipitated calcium carbonate and bentonite mixtures after drying, and modifying agent is weight ratio
For poly- naphthalene formaldehyde sulfonate salt, polyethylene glycol and the isopropanolamine of 1:1-3:0.5-1.
Further, in the raw material of the adhesive layer, the tackifier are coumarone resin, and the antioxidant is Asia
Tricresyl phosphate (2,4- di-tert-butyl-phenyl) ester, the plasticizer are dibutyl phthalate (DBP), trimellitic acid rouge or epoxy soybean
One of oil；The crosslinking agent is vinyltriethoxysilane, vinyl three (β-methoxy ethoxy) silane, ethylene
Base triacyloxysilanes, three tert-butoxy vinyl silanes or vinyl silane tri-butyl peroxy, the crosslinking accelerator are
3-aminopropyltriethoxysilane.
Further, in the raw material of the polyolefin thermoplastic elastomer, the antioxidant is thio-2 acid two (12
Alcohol) ester or thio-2 acid two (octadecyl alcolol) ester；Age resister is 2,6 di tert butyl 4 methyl phenol；Softening agent is to subtract two
Line machine oil or the line machine oil that subtracts three.
The present invention also provides the preparation methods of above-mentioned reaction bonded wet-laying polymer membranes, comprising the following steps:
(1) in parts by weight by the copolymer of polyisobutene, ethylene and octene, antioxidant, age resister, softening agent, fill out
Charge is mediated in 120 DEG C~180 DEG C of at a temperature of mixing to being uniformly mixed, and modified polypropene is then added, 180 DEG C~210
The second mixing is carried out at a temperature of DEG C, squeezes out to obtain polyolefin thermoplastic elastomer film through extruder；
(2) 90# asphalt is added in reaction heating kettle according to parts by weight, reaction temperature is heated to 145~
After 165 DEG C, crosslinking agent is added, is stirred 60~90 minutes with high-speed shearing machine, then heats to 175~180 DEG C, in a kettle
Sequentially add tackifier, plasticizer, high-speed shearing machine stirring 40~after sixty minutes, it is anti-oxidant to be cooled to 145~165 DEG C of additions
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in agent, filler material；
(3) under conditions of 150-180 DEG C, by modified oil pitch binder and the hot pressing of polyolefin thermoplastic elastomer film
Bonding controls thick sizing and covers isolation film protective layer, winding is made.
Wherein it is preferred in step (1), control the polyolefin thermoplastic elastomer film (1) with a thickness of 0.5~
2.0mm。
Wherein it is preferred to which isolation film protective layer is polyethylene film, polychloroethylene film or polyester film.
In the present invention, mainly by asphalt, tackifier, plasticizer, antioxidant, crosslinking agent, crosslinking promotees adhesive layer
It is prepared into agent, filler material.The plasticizer of addition can weaken the aggtegation of molecule interchain, can dramatically increase asphalt
Low temperature flexibility and heat-resisting quantity；Tackifier can significantly improve the viscosity and thermostabilization of asphalt using coumarone resin
Property, increase its cementability between base；The chemical stability of adhesive layer can be improved in antioxidant, prevents its aging；It adopts
Crosslinking agent and crosslinking accelerator can be chemically reacted with cast-in-place concrete, between the two the shape under catalyst system effect
At chemical bond, make coiled material securely in conjunction with concrete or cement interface；In the curing process, consumption is a large amount of for cement simultaneously
Water leads to the curing exotherm for generating negative pressure and cement in the system for forming partial closure between cement and self-adhesive coiled material, promotes
The creep of self-adhesive, is deep into it in capillary or hole of concrete, forms the effect of physics mortise and tenon, reaches reliable bonding
Effect；While self-adhesive oxidant layer is penetrated into the capillary or hole of concrete, increase what self-adhesive was contacted with concrete
Area promotes self-adhesive oxidant layer and concrete to form more ionic bonds, and plays " chemical crosslinking-physics mortise and tenon collaboration effect
Answer " (Chemical Bonding and Physical Crosslinking Synergism, abbreviation CPS), make basal plane and oneself
Adhesion coating forms " interpenetrating networks formula " interfacial structure, to keep bonding more firm, enables it to thoroughly solve to ask with what base bonded
The problem of topic and wet surface construction.Therefore, adhesive layer of the present invention passes through the compounding of each component and each component content, can significantly mention
Low temperature flexibility, thermal stability and the cohesive force of high adhesive layer of the present invention, adhesive layer can also occur chemistry with concrete and hand over
Connection-physics mortise and tenon synergistic effect, acquisition are used in mixed way bigger cementation power than pitch and crosslinking agent, reach more preferably close
Seal waterproof effect.
Polyolefin thermoplastic elastomer is one kind by polypropylene, polyethylene and the resulting polymerization of EP rubbers blending reaction
Object, after antioxidant, anti-aging agent, softening agent is added, with anti-aging, tensile strength is high, the big advantage of elongation.This material is not
It is simple blend, but an equally distributed copolymerization continuous phase, there are a series of unique performances, not because of its raw material
Together, the performance of product can have significant difference.It in the present invention, is found by experiment that, uses molecular weight for 10,000~100,000
Polyisobutene, the ethylene that molecular weight is 1000~3500 and copolymer, the EP rubbers of octene mix according to a certain percentage,
Then modified polypropene, antioxidant, age resister, softening agent, filler material is added, can obtain that tensile strength is higher, cracking resistance
Better polyolefin thermoplastic elastomer basement membrane.It the polyacrylic surface of polyolefin thermoplastic elastomer basement membrane can low, wetability
Poor, low polarity so that its as material as tire base when, it is low with the adhesive force of adhesive phase, as paved surface generate crack, tire
There is the possibility peeled off and then be broken in base, and influences the sealing performance of coiled material, and the present invention uses chlorinated polypropylene and aphthenic acids
Zinc catalyst is 50,000~300,000 polypropylene modification to average molecular weight, can improve that its low-surface-energy is low, low polar spy
Property, increase the wetability of polyolefin thermoplastic elastomer basement membrane and the adhesive force with adhesive phase, to ensure waterproof seal
It can more persistently.Filler material be the precipitated calcium carbonate that mass ratio is 1-3:6 and bentonite it is mixed and modified after mixture, modification disappear
It in addition to calcium carbonate and bentonite itself freely agglomerate, so that its partial size is more preferable, more uniformly spreads, thus in polyolefin thermoplastic
Property elastomer in mixedly more uniformly, guarantee tire base intensity.Though and bentonite good dispersion itself, itself and cement water
Effective corresponding circle of sensation cannot be formed or strengthen transition region by closing between mineral, be easy to cause infiltration, and the present invention, which passes through, uses poly- naphthalene first
Aldehyde sulfonate sodium, polyethylene glycol and isopropanolamine are modified it, while ensure that its good dispersibility, keep it mixed in cement
It can play the role of effective water proof anti-seepage in solidifying soil, not influence waterproof seal of the invention.In addition, this polyolefine thermoplastic elastomer
Filler additive amount in body basement membrane has a significant effect to the elongation percentage of basement membrane, tensile strength and tearing strength, adds in of the invention
Within the scope of dosage, it is able to maintain preferable performance, and improve significantly to the anti-ageing property of this polyolefin thermoplastic elastomer basement membrane
Effect.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1, reaction bonded wet-laying polymer membranes of the invention, passes through the compounding of each component and each component content, energy
The low temperature flexibility, thermal stability and cohesive force of adhesive layer of the present invention are enough significantly improved, adhesive layer can also be sent out with concrete
Biochemical crosslinking-physics mortise and tenon synergistic effect, acquisition are used in mixed way bigger cementation power than pitch and crosslinking agent, reach
More preferably sealed waterproof effect.
2, the present invention in polyolefin thermoplastic elastomer using specified molecular weight polyisobutene, ethylene and octene copolymerization
Object and modified polypropene and EP rubbers are major ingredient, have better molecular chain structure after mixing, high with tensile strength,
The advantage that elongation is big and cracking resistance is good, polyacrylic modification is so that polyolefin thermoplastic elastomer film has preferably wetting
Property and adhesion guarantee the sealing waterproof performance of material, are being laid with to can occur with adhesive phase closer bonding
When face generates crack, avoids that base's fracture or base occurs and adhesive layer is layered, ensure that the waterproof sealing effect of coiled material.
3, polyolefine thermoplastic elastomer control filling kind and dosage in the present invention, ensure that preferable elongation percentage, stretching
Intensity and tearing strength, and the anti-ageing property of polyolefin thermoplastic elastomer basement membrane can be made to improve significantly.
[specific embodiment]
In order to more clearly express the present invention, below by way of specific embodiment, the invention will be further described.
Embodiment 1
A kind of reaction bonded wet-laying polymer membranes, including be located at upper layer polyolefin thermoplastic elastomer base,
It is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, specifically:
Adhesive layer is prepared from the following raw materials: asphalt 55kg, tackifier coumarone resin 7kg, plasticizer neighbour benzene two
Formic acid dibutylester 5kg, antioxidant phosphorous acid three (2,4- di-tert-butyl-phenyl) ester 0.5kg, crosslinking agent vinyl triethoxyl
Silane, 0.5kg, crosslinking accelerator 3-aminopropyltriethoxysilane 0.2kg, filler material 20kg；
Polyolefin thermoplastic elastomer is prepared from the following raw materials: the polyisobutene that molecular weight is 10,000~100,000
5kg, the copolymer 20kg of the ethylene that molecular weight is 1000~3500 and octene, EP rubbers 3kg, modified polypropene 10kg, resist
Two (lauryl alcohol) ester 1.2kg of oxygen agent thio-2 acid, age resister 2,6 di tert butyl 4 methyl phenol 1.0kg, softening agent
1kg, filler material 20kg；
The present invention also provides the preparation methods of above-mentioned reaction bonded wet-laying polymer membranes, comprising the following steps:
(1) pretreatment of raw material:
Modified polypropene: average molecular weight of making even be 50,000~300,000 polypropylene 50kg, chlorinated polypropylene 20kg,
Zinc naphthenate catalyst 3kg, 120 DEG C at a temperature of be stirred to react 20min, be then granulated into particulate matter.
Modified alta-mud: poly- naphthalene formaldehyde sulfonate salt, polyethylene glycol and isopropanolamine are got out by weight for 1:1:0.5
It is spare as modifying agent；It is dry by weight taking precipitated calcium carbonate and bentonite mixtures to be dehydrated under conditions of 110 DEG C for 1~3
It is dry, it is then added in high-speed mixer, modifying agent is added into mixture under conditions of 75 DEG C, in the high speed of 1000r/min
The lower modified 15min of stirring, obtains filler material；Wherein the dosage of modifying agent is the precipitated calcium carbonate and bentonite mixtures after drying
2.5%.
(2) prepare polyolefin thermoplastic elastomer film: in parts by weight by the copolymer of polyisobutene, ethylene and octene,
Antioxidant, age resister, softening agent, filler material are mediated in 120 DEG C of at a temperature of mixing to being uniformly mixed, and are then added modified poly-
Propylene, 180 DEG C at a temperature of carry out the second mixing, squeeze out to obtain polyolefin thermoplastic elastomer film through extruder, control is poly-
Olefinic thermoplastic elastomer film thickness is 1.5mm.
(3) it prepares modified oil pitch binder: 90# asphalt being added to reaction heating kettle according to parts by weight
In, after reaction temperature is heated to 158 DEG C, crosslinking agent is added, is stirred 60 minutes with high-speed shearing machine, then heats to 175 DEG C,
Tackifier, plasticizer are sequentially added in a kettle, and high-speed shearing machine stirs after forty minutes, and it is anti-oxidant to be cooled to 145 DEG C of additions
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in agent, filler material；
(4) compound: under conditions of 150 DEG C, by modified oil pitch binder and polyolefin thermoplastic elastomer film heat
Pressure viscosity knot controls thick sizing and covers isolation film protective layer, winding is made.Isolation film protective layer be polyethylene film, polychloroethylene film or
Polyester film.
Embodiment 2
A kind of reaction bonded wet-laying polymer membranes, including be located at upper layer polyolefin thermoplastic elastomer base,
It is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, specifically:
Adhesive layer is prepared from the following raw materials: asphalt 58kg, tackifier coumarone resin 8kg, the inclined benzene three of plasticizer
Sour rouge 8kg, antioxidant phosphorous acid three (2,4- di-tert-butyl-phenyl) ester 0.7kg, (β-methoxyl group second of crosslinking agent vinyl three
Oxygroup) silane 1.2kg, crosslinking accelerator 3-aminopropyltriethoxysilane 0.5kg, filler material 25kg；
Polyolefin thermoplastic elastomer is prepared from the following raw materials: the polyisobutene that molecular weight is 10,000~100,000
8kg, the ethylene that molecular weight is 1000~3500 and the copolymer 25kg of octene, EP rubbers 4.5kg, modified polypropene 18kg,
(lauryl alcohol) ester of antioxidant thio-2 acid two 1.6kg, age resister 2,6 di tert butyl 4 methyl phenol 1.5kg, softening agent
2kg, filler material 24kg；
The present invention also provides the preparation methods of above-mentioned reaction bonded wet-laying polymer membranes, comprising the following steps:
(2) pretreatment of raw material:
Modified polypropene: average molecular weight of making even be 50,000~300,000 polypropylene 55kg, chlorinated polypropylene 25kg,
Zinc naphthenate catalyst 4kg, 150 DEG C at a temperature of be stirred to react 30min, be then granulated into particulate matter.
Modified alta-mud: poly- naphthalene formaldehyde sulfonate salt, polyethylene glycol and isopropanolamine are got out by weight for 1:2:0.8
It is spare as modifying agent；Precipitated calcium carbonate and bentonite mixtures are taken to take off under conditions of 110~120 DEG C by weight for 1~5
Water is dry, is then added in high-speed mixer, modifying agent is added into mixture under conditions of 80 DEG C, 1200r/min's
Modified 12min, obtains filler material under high-speed stirred；Wherein the dosage of modifying agent is that precipitated calcium carbonate and bentonite after drying mix
Close the 2.8% of object.
(2) prepare polyolefin thermoplastic elastomer film: in parts by weight by the copolymer of polyisobutene, ethylene and octene,
Antioxidant, age resister, softening agent, filler material are mediated in 150 DEG C of at a temperature of mixing to being uniformly mixed, and are then added modified poly-
Propylene, 200 DEG C at a temperature of carry out the second mixing, squeeze out to obtain polyolefin thermoplastic elastomer film through extruder, control is poly-
Olefinic thermoplastic elastomer film thickness is 1.5mm.
(3) it prepares modified oil pitch binder: 90# asphalt being added to reaction heating kettle according to parts by weight
In, after reaction temperature is heated to 150 DEG C, crosslinking agent is added, is stirred 70 minutes with high-speed shearing machine, then heats to 176 DEG C,
Tackifier, plasticizer are sequentially added in a kettle, and it is anti-oxidant to be cooled to 158 DEG C of additions after high-speed shearing machine stirs 45 minutes
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in agent, filler material；
(4) compound: under conditions of 160 DEG C, by modified oil pitch binder and polyolefin thermoplastic elastomer film heat
Pressure viscosity knot controls thick sizing and covers isolation film protective layer, winding is made.Isolation film protective layer be polyethylene film, polychloroethylene film or
Polyester film.
Embodiment 3
A kind of reaction bonded wet-laying polymer membranes, including be located at upper layer polyolefin thermoplastic elastomer base,
It is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, specifically:
Adhesive layer is prepared from the following raw materials: asphalt 59kg, tackifier coumarone resin 9kg, plasticizer epoxy are big
Soya-bean oil 7kg, antioxidant phosphorous acid three (2,4- di-tert-butyl-phenyl) 0.5~1kg of ester, three tert-butoxy vinyl silicon of crosslinking agent
Alkane 1.0kg, crosslinking accelerator 3-aminopropyltriethoxysilane 0.5kg, filler material 26kg；
Polyolefin thermoplastic elastomer is prepared from the following raw materials: the polyisobutene that molecular weight is 10,000~100,000
7kg, the copolymer 22kg of the ethylene that molecular weight is 1000~3500 and octene, EP rubbers 4kg, modified polypropene 18kg, resist
Two (octadecyl alcolol) ester 1.8kg of oxygen agent thio-2 acid, age resister 2,6 di tert butyl 4 methyl phenol 1.6kg, softening agent
2.3kg, filler material 28kg；
The present invention also provides the preparation methods of above-mentioned reaction bonded wet-laying polymer membranes, comprising the following steps:
(3) pretreatment of raw material:
Modified polypropene: average molecular weight of making even be 50,000~300,000 polypropylene 65kg, chlorinated polypropylene 28kg,
Zinc naphthenate catalyst 4kg, 185 DEG C at a temperature of be stirred to react 32min, be then granulated into particulate matter.
Modified alta-mud: poly- naphthalene formaldehyde sulfonate salt, polyethylene glycol and isopropanolamine are got out by weight for 1:2:0.9
It is spare as modifying agent；It is dry by weight taking precipitated calcium carbonate and bentonite mixtures to be dehydrated under conditions of 118 DEG C for 1~5
It is dry, it is then added in high-speed mixer, modifying agent is added into mixture under conditions of 85 DEG C, in the high speed of 1250r/min
The lower modified 12min of stirring, obtains filler material；Wherein the dosage of modifying agent is the precipitated calcium carbonate and bentonite mixtures after drying
2.8%.
(2) prepare polyolefin thermoplastic elastomer film: in parts by weight by the copolymer of polyisobutene, ethylene and octene,
Antioxidant, age resister, softening agent, filler material are mediated in 170 DEG C of at a temperature of mixing to being uniformly mixed, and are then added modified poly-
Propylene, 200 DEG C at a temperature of carry out the second mixing, squeeze out to obtain polyolefin thermoplastic elastomer film through extruder, control is poly-
Olefinic thermoplastic elastomer film thickness is 1.5mm.
(3) it prepares modified oil pitch binder: 90# asphalt being added to reaction heating kettle according to parts by weight
In, after reaction temperature is heated to 160 DEG C, crosslinking agent is added, is stirred 75 minutes with high-speed shearing machine, then heats to 178 DEG C,
Tackifier, plasticizer are sequentially added in a kettle, and it is anti-oxidant to be cooled to 162 DEG C of additions after high-speed shearing machine stirs 55 minutes
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in agent, filler material；
(4) compound: under conditions of 170 DEG C, by modified oil pitch binder and polyolefin thermoplastic elastomer film heat
Pressure viscosity knot controls thick sizing and covers isolation film protective layer, winding is made.Isolation film protective layer be polyethylene film, polychloroethylene film or
Polyester film.
Embodiment 4
A kind of reaction bonded wet-laying polymer membranes, including be located at upper layer polyolefin thermoplastic elastomer base,
It is located in the middle modified pitch adhesive layer and the isolation film protective layer positioned at lower layer, specifically:
Adhesive layer is prepared from the following raw materials: asphalt 60kg, tackifier coumarone resin 10kg, plasticizer neighbour benzene two
Formic acid dibutylester 10kg, antioxidant phosphorous acid three (2,4- di-tert-butyl-phenyl) ester 1kg, crosslinking agent vinyl tri-tert mistake
Oxosilane 2kg, crosslinking accelerator 3-aminopropyltriethoxysilane 0.6kg, filler material 30kg；
Polyolefin thermoplastic elastomer is prepared from the following raw materials: the polyisobutene that molecular weight is 10,000~100,000
10kg, the copolymer 30kg of the ethylene that molecular weight is 1000~3500 and octene, EP rubbers 6kg, modified polypropene 25kg, resist
Two (lauryl alcohol) ester of oxygen agent thio-2 acid or (octadecyl alcolol) ester of thio-2 acid two 2.0kg, age resister 2,6- di-t-butyl-
4- methylphenol 2.0kg, softening agent 3kg, filler material 30kg；
The present invention also provides the preparation methods of above-mentioned reaction bonded wet-laying polymer membranes, comprising the following steps:
(4) pretreatment of raw material:
Modified polypropene: average molecular weight of making even be 50,000~300,000 polypropylene 70kg, chlorinated polypropylene 30kg,
Zinc naphthenate catalyst 5kg, 210 DEG C at a temperature of be stirred to react 20min, be then granulated into particulate matter.
Modified alta-mud: make by weight poly- naphthalene formaldehyde sulfonate salt, polyethylene glycol and isopropanolamine is got out for 1:3:1
It is spare for modifying agent；Precipitated calcium carbonate and bentonite mixtures are taken to dehydrate under conditions of 120 DEG C by weight for 1~6,
It is then added in high-speed mixer, modifying agent is added into mixture under conditions of 90 DEG C, in the high-speed stirred of 1300r/min
Lower modified 15min, obtains filler material；Wherein the dosage of modifying agent is the precipitated calcium carbonate and bentonite mixtures after drying
3.0%.
(2) prepare polyolefin thermoplastic elastomer film: in parts by weight by the copolymer of polyisobutene, ethylene and octene,
Antioxidant, age resister, softening agent, filler material are mediated in 180 DEG C of at a temperature of mixing to being uniformly mixed, and are then added modified poly-
Propylene, 210 DEG C at a temperature of carry out the second mixing, squeeze out to obtain polyolefin thermoplastic elastomer film through extruder, control is poly-
Olefinic thermoplastic elastomer film thickness is 1.5mm.
(3) it prepares modified oil pitch binder: 90# asphalt being added to reaction heating kettle according to parts by weight
In, after reaction temperature is heated to 165 DEG C, crosslinking agent is added, is stirred 90 minutes with high-speed shearing machine, then heats to 180 DEG C,
Tackifier, plasticizer are sequentially added in a kettle, and high-speed shearing machine stirs after sixty minutes, and it is anti-oxidant to be cooled to 165 DEG C of additions
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in agent, filler material；
(4) compound: under conditions of 180 DEG C, by modified oil pitch binder and polyolefin thermoplastic elastomer film heat
Pressure viscosity knot controls thick sizing and covers isolation film protective layer, winding is made.Isolation film protective layer be polyethylene film, polychloroethylene film or
Polyester film.
Comparative example 1
The comparative example 1 the difference from example 2 is that modified polypropene use average molecular weight for 400,000 or more not
Modified polypropylene replaces.
Comparative example 2
The comparative example 1 is the difference from example 2 is that filler material is replaced using untreated precipitated calcium carbonate.
Comparative example 3
The comparative example 1 is the difference from example 2 is that the dosage of filler material is 35kg.
Embodiment 1-4 and comparative example 1-3 are prepared into resulting waterproof roll according to GB/T35467-2017 " wet-laying waterproof
Coiled material " it is tested for the property, test result sees below Tables 1 and 2.
Table 2
The waterproof roll performance that can be seen that 1-4 of the embodiment of the present invention from the result of Tables 1 and 2 has been more than national mark
Alignment request, performance are very excellent.Adhesive property between comparative example 1 and concrete is also very good, but it is due to polyolefin thermoplastic
Property elastomer film fracture when be layered, in use, if paved surface generate crack when, it may occur however that base
It is layered with adhesive layer, causes to seep water.The filler material used in comparative example 1 is untreated, affects the dispersibility of system, makes
It obtains its mechanical property such as tensile property and tear resistance and is all worse than the present invention, and the filler material in its comparative example 2 is free of bentonite,
Its anti-ageing property is also worse than the present invention, illustrates bentonite after modified, has synergistic effect to anti-ageing property is improved.In comparative example 3 because
Filler material excessive addition to a certain extent also reduces the partial properties of product.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the patents of the present invention.
Claims (8)
1. a kind of reaction bonded wet-laying polymer membranes, polyolefin thermoplastic elastomer base, position including being located at upper layer
In intermediate modified pitch adhesive layer and positioned at the isolation film protective layer of lower layer, it is characterised in that:
The adhesive layer is mainly made of raw material from the following weight: 55~60 parts of asphalt, increases 7~10 parts of tackifier
Mould 5~10 parts of agent, 0.5~1 part of antioxidant, 0.5~2 part of crosslinking agent, 0.2~0.6 part of crosslinking accelerator, filler material 20~30
Part；
The polyolefin thermoplastic elastomer is mainly made of raw material from the following weight: molecular weight is 10,000~100,000
5~10 parts of polyisobutene, molecular weight be 1000~3500 ethylene and octene 20~30 parts of copolymer, EP rubbers 3~6
Part, 10~25 parts of modified polypropene, 1.2~2.0 parts of antioxidant, 1.0~2.0 parts of age resister, 1~3 part of softening agent, filler material
20~30 parts；Wherein, the filler material be precipitated calcium carbonate that mass ratio is 1-3:6 and bentonite it is mixed and modified after mixing
Object.
2. a kind of reaction bonded wet-laying polymer membranes according to claim 1, it is characterised in that: the modification is poly-
Propylene is to be prepared by the following method and obtain: average molecular weight of making even be 50,000~300,000 50~70 parts of polypropylene, chlorination
20~30 parts of polypropylene, 3~5 parts of zinc naphthenate catalyst, 120 DEG C~210 DEG C at a temperature of be stirred to react 20~40min,
Then it is granulated into particulate matter.
3. a kind of reaction bonded wet-laying polymer membranes according to claim 1, it is characterised in that: the modification is swollen
Profit soil is prepared by the following method to obtain: taking the condition of precipitated calcium carbonate and bentonite mixtures at 110~120 DEG C by weight
Lower dehydration and drying, is then added in high-speed mixer, and modifying agent, In are added into mixture under conditions of 75~90 DEG C
Modified 10~15min, obtains filler material under the high-speed stirred of 1000-1300r/min；After wherein the dosage of modifying agent is dry
The 2.5-3.0% of precipitated calcium carbonate and bentonite mixtures, modifying agent are the poly- naphthaldehyde sulfonic acid that weight ratio is 1:1-3:0.5-1
Sodium salt, polyethylene glycol and isopropanolamine.
4. a kind of reaction bonded wet-laying polymer membranes according to claim 1, it is characterised in that: the binder
In the raw material of layer, the tackifier are coumarone resin, and the antioxidant is phosphorous acid three (2,4- di-tert-butyl-phenyl) ester,
The plasticizer is one of dibutyl phthalate (DBP), trimellitic acid rouge or epoxidized soybean oil；The crosslinking agent is ethylene
Ethyl triethoxy silicane alkane, vinyl three (β-methoxy ethoxy) silane, vinyl triacyloxysilanes, three tert-butoxy second
Alkenyl silanes or vinyl silane tri-butyl peroxy, the crosslinking accelerator are 3-aminopropyltriethoxysilane.
5. a kind of reaction bonded wet-laying polymer membranes according to claim 1, it is characterised in that: the polyolefin
In the raw material of thermoplastic elastomer (TPE), the antioxidant is (lauryl alcohol) ester of thio-2 acid two or thio-2 acid two (octadecyl alcolol)
Ester；Age resister is 2,6 di tert butyl 4 methyl phenol；Softening agent is second line of distillation machine oil or the line machine oil that subtracts three.
6. the preparation method of reaction bonded wet-laying polymer membranes of any of claims 1-5, feature exist
In, comprising the following steps:
(1) in parts by weight by the copolymer of polyisobutene, ethylene and octene, antioxidant, age resister, softening agent, filler material
It mediates in 120 DEG C~180 DEG C of at a temperature of mixing to being uniformly mixed, modified polypropene is then added, at 180 DEG C~210 DEG C
At a temperature of carry out the second mixing, squeeze out to obtain polyolefin thermoplastic elastomer film through extruder；
(2) 90# asphalt is added in reaction heating kettle according to parts by weight, reaction temperature is heated to 145~165 DEG C
Afterwards, crosslinking agent is added, is stirred 60~90 minutes with high-speed shearing machine, then heats to 175~180 DEG C, in a kettle successively
Addition tackifier, plasticizer, high-speed shearing machine stirring 40~after sixty minutes, it is cooled to 145~165 DEG C of addition antioxidants, fills out
Modified oil pitch binder is made until 90# asphalt is uniformly dispersed with unclassified stores in charge；
(3) under conditions of 150-180 DEG C, modified oil pitch binder and polyolefin thermoplastic elastomer film hot pressing are glued
Knot controls thick sizing and covers isolation film protective layer, winding is made.
7. the preparation method of reaction bonded wet-laying polymer membranes according to claim 6, it is characterised in that: step
(1) in, the polyolefin thermoplastic elastomer film (1) is controlled with a thickness of 0.5~2.0mm.
8. the preparation method of reaction bonded wet-laying polymer membranes according to claim 6, it is characterised in that: isolation
Film protective layer is polyethylene film, polychloroethylene film or polyester film.
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