CN109514964A - A kind of preparation method of modified asphalt waterproof coiled material - Google Patents
A kind of preparation method of modified asphalt waterproof coiled material Download PDFInfo
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- CN109514964A CN109514964A CN201811467897.3A CN201811467897A CN109514964A CN 109514964 A CN109514964 A CN 109514964A CN 201811467897 A CN201811467897 A CN 201811467897A CN 109514964 A CN109514964 A CN 109514964A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/08—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the cooling method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0004—Cutting, tearing or severing, e.g. bursting; Cutter details
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
- C08G83/006—After treatment of hyperbranched macromolecules
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The present invention relates to waterproof roll fields, propose a kind of preparation method of modified asphalt waterproof coiled material.The preparation method of above-mentioned modified asphalt waterproof coiled material, comprising the following steps: prepare diisopropanolamine (DIPA) mixed solution, prepare trimellitic acid anhydride solution；By diisopropanolamine (DIPA) mixed solution and trimellitic anhydride solution mixing system for AB2Monomer mixed solution；In AB2Triethanolamine, toluenesulfonic acid and water entrainer are added in monomer mixed solution, dissaving polymer solution is made after reaction；Modified end dissaving polymer is made after being reacted, being evaporated under reduced pressure after methyl acrylate and toluenesulfonic acid mixing is added；Continuously add the obtained modified pitch such as bitumen base；Waterproof roll is made using modified pitch.The preparation method of above-mentioned modified asphalt waterproof coiled material utilizes dissaving polymer modified synergic pitch together with SBS, so that cost is lower, and does not need prolonged high temperature grinding in the manufacturing process of waterproof roll, technique is simpler.
Description
Technical field
The present invention relates to waterproof roll fields, in particular to a kind of preparation method of modified asphalt waterproof coiled material.
Background technique
SBS modified asphalt waterproof coiled material is the widest waterproof roll of domestic application, and dosage is big, wide coverage.Raw material
In the SBS that uses be styrene-butadiene-styrene triblock copolymer, be a kind of thermoplastic elastomer (TPE), and the price of SBS
It is very expensive, make the price of waterproof roll also high accordingly.
Dissaving polymer is that one kind is similar to dendritic, but its intramolecule existing defects, is not completely right
Claim the polymer of spherical structure.Dissaving polymer is usually by the AB containing two kinds of reactive groups of A, B x Type (x>=2) list
What body was prepared.Dissaving polymer shows as elliposoidal, has three-dimensional structure.Due to the structure of dissaving polymer
Feature, solvability, viscosity, in terms of have excellent performance.Currently, dissaving polymer is applying
Material, polymer film, pharmaceutical carrier, fire retardant etc. are widely used.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of modified asphalt waterproof coiled material, utilize dissaving polymer
The modified synergic pitch together with SBS.Compared with the independent modified pitch of traditional SBS, cost is lower, and can be good at lower
At a temperature of be directly dissolved in pitch.Also, it does not need to pass through prolonged high temperature as SBS in the manufacturing process of waterproof roll
Grinding, preparation process are simpler.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of modified asphalt waterproof coiled material comprising following steps:
Step S1: by diisopropanolamine (DIPA), initiator, magnetic Fe3O4Microballoon and organic solvent are mixed to prepare the dense of diisopropanolamine (DIPA)
Degree be 1~1.5mol/L diisopropanolamine (DIPA) mixed solution, organic solvent be n,N-dimethylacetamide, dimethylformamide and
At least one of cyclohexanone；
Step S2: in organic solvent by trimellitic anhydride dissolution, it is molten that the trimellitic anhydride that concentration is 1~1.5mol/L is made
Liquid；
Diisopropanolamine (DIPA) mixed solution: being added in trimellitic acid anhydride solution by step S3 under inert gas protection, and super
4~6h is reacted under the conditions of sound under the conditions of 35~45 DEG C, AB is made2Monomer mixed solution；
Step S4: in AB2Triethanolamine, toluenesulfonic acid and water entrainer are added in monomer mixed solution, in 140~145 DEG C of temperature models
Enclose interior prepared by microwave reaction dissaving polymer solution；
Step S5: it is 88~92 DEG C in temperature after dissaving polymer solution, methyl acrylate and toluenesulfonic acid are mixed and condenses
Modified end dissaving polymer solution is made in 5~7h reaction that flows back, and the modified hyperbranched polymerization in end is made after being evaporated under reduced pressure
Object；
Step S6: after 20~40min is mixed in bitumen base, softening auxiliary agent, addition SBS, graphene, modified end are super
Branched polymer reacts 1~3h under the conditions of 170~185 DEG C and reaction mixture is made；Reaction mixture, talcum powder are mixed equal
It is even, add age resister, toughener is stirred to react 1~2h and modified pitch is made；
Step S7: respectively coating one layer of modified pitch for nonwoven layer tire base upper and lower surfaces and obtain modified asphalt layer, drips modified
Cyan layer surface bonds PE film, through cooling, meter length, trimming and winds obtained waterproof roll.
The beneficial effect of the preparation method of the modified asphalt waterproof coiled material of the embodiment of the present invention is: first preparing hyperbranched polymerization
Object recycles above-mentioned dissaving polymer with SBS together modified synergic pitch, finally prepares modified asphalt waterproof coiled material.Firstly,
The preparation method of above-mentioned modified asphalt waterproof coiled material is compared with the independent modified pitch of traditional SBS, because controlling costly
SBS dosage, so cost is lower.Secondly, dissaving polymer can be good at being directly dissolved in drip at a lower temperature
Blueness, so that the pitch of synthesis has preferable performance.Again, it does not need to pass through as SBS in the manufacturing process of waterproof roll
Prolonged high temperature grinding, preparation process are simpler.Finally, joined magnetic Fe in the raw material of reaction 3O 4Microballoon simultaneously leads to
The modified asphalt waterproof coiled material that microwave reaction is prepared is crossed to have excellent performance.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The properties such as the excellent solvability of dissaving polymer make dissaving polymer apply the manufacture in waterproof roll
It does not need to pass through prolonged high temperature grinding as SBS in the process, and can be good at being directly dissolved at a lower temperature
Pitch.And dissaving polymer is more saved in cost with SBS modified synergic pitch.
Graphene is a kind of typical two-dimension netted material, and grapheme material is applied in waterproof roll, can be effective
Raising waterproof roll stability, performances such as heat-resisting, ageing-resistant, and can significantly improve the service life of graphene.
The mode of graphene is added during preparing material, graphene is enabled to be uniformly distributed in the material.
A kind of infant formula goat milk powder of the embodiment of the present invention and preparation method thereof is specifically described below.
The present invention provides a kind of preparation methods of modified asphalt waterproof coiled material, comprising the following steps:
Step S1: by diisopropanolamine (DIPA), initiator, magnetic Fe 3O 4Microballoon and organic solvent are mixed to prepare the dense of diisopropanolamine (DIPA)
Degree be 1~1.5mol/L diisopropanolamine (DIPA) mixed solution, organic solvent be n,N-dimethylacetamide, dimethylformamide and
At least one of cyclohexanone；In preparation AB2Solution preparation is carried out before monomer mixed solution, in process for preparation, in diisopropanol
Initiator is added in mixing in amine, can effectively improve AB2The conversion ratio of the technique of monomer synthesis.Magnetic Fe3O4Microballoon is as magnetic
Property substance, be capable of effectively it is subsequent enhancing microwave effect so that obtained modified asphalt waterproof coiled material performance is more excellent.
Further, in a preferred embodiment of the present invention, diisopropanolamine (DIPA), initiator and magnetic in preparation method step S1
Property Fe3O4The amount ratio of microballoon be 0.100~0.110mol:0.001~0.002mol:0.001~0.002mol:0.1~
0.2g。AB2Yield is lower during the preparation process for monomer.If in AB2During monomer synthesizes, magnetic Fe is added3O4Microballoon can
Positive effect is played in subsequent microwave reaction, so that the final product modified asphalt waterproof coiled material effect that reaction obtains is more
It is good.It is that modified asphalt waterproof coiled material effect obtained is the most excellent when the ratio of above-mentioned substance is aforementioned proportion.
Step S2: in organic solvent by trimellitic anhydride dissolution, the trimellitic anhydride that concentration is 1~1.5mol/L is made
Solution；
Diisopropanolamine (DIPA) mixed solution: being added in trimellitic acid anhydride solution by step S3 under inert gas protection, and super
4~6h is reacted under the conditions of sound under the conditions of 35~45 DEG C, AB is made2Monomer mixed solution；Above-mentioned time, AB are reacted at the temperature disclosed above2
The yield of monomer is higher, and from the point of view of binding time cost and cost of energy, more saves.
Further, in a preferred embodiment of the present invention, the intensity of ultrasonic treatment is 40~50Hz.In preparation AB2Monomer
During mixed liquor, carries out ultrasonic treatment and enable to AB2The yield of monomer is higher.The AB of synthesis2Monomer yield is higher, system
The performance of standby modified asphalt waterproof coiled material is more preferable.
Further, in a preferred embodiment of the present invention, the diisopropanolamine (DIPA) and trimellitic acid in diisopropanol amine aqueous solution
The amount ratio of trimellitic anhydride in anhydride solution is 1mol:1~1.1mol.It is synthesized using diisopropanolamine (DIPA) and trimellitic anhydride
AB2During monomer, theoretically the two is that 1:1 is reacted, but is found after having carried out some experiments with molar ratio
Trimellitic anhydride can excessively improve AB to a certain extent2The yield of monomer.
Step S4: in AB2Triethanolamine, toluenesulfonic acid and water entrainer are added in monomer mixed solution, in 140~145 DEG C of temperature
Spend prepared by microwave reaction dissaving polymer solution in range；During preparing dissaving polymer, three ethyl alcohol of addition
Amine can effectively improve the conversion ratio of polymerization reaction as catalyst as core molecule, toluenesulfonic acid.Meanwhile in reaction process
Middle addition water entrainer can timely take away moisture obtained in reaction process, accelerate the rate that reaction carries out.Very much
In Practical in Chemistry, microwave reaction can generate more positive effect to the final result of chemical reaction, thus it is micro- to be also born
The knowledge hierarchy of wave chemistry.In this step in the lower carry out polymerization reaction of microwave condition, turning for reaction can be effectively improved
Rate.
Further, in a preferred embodiment of the present invention, water entrainer is one of toluene or benzene.
Further, in a preferred embodiment of the present invention, AB2Monomer mixed solution, triethanolamine, toluenesulfonic acid and water entrainer
Amount ratio be 100ml:0.004~0.006mol:0.140~0.180g:75~80ml.It is polymerize using being combined when aforementioned proportion
The conversion ratio of reaction is higher.
Further, in a preferred embodiment of the present invention, the microwave intensity of microwave reaction is 2000~2300MHz.
Step S5: by dissaving polymer solution, methyl acrylate and toluenesulfonic acid mix after temperature be 88~92 DEG C
It is condensed back 5~7h reaction and modified end dissaving polymer solution is made, it is hyperbranched that modified end is made after being evaporated under reduced pressure
Polymer；
Step S6: after 20~40min is mixed in bitumen base, softening auxiliary agent, addition SBS, graphene, modified end are super
Branched polymer reacts 1~3h under the conditions of 170~185 DEG C and reaction mixture is made；Reaction mixture, talcum powder are mixed equal
It is even, add age resister, toughener is stirred to react 1~2h and modified pitch is made；
Further, in a preferred embodiment of the present invention, in parts by weight, bitumen base is 75~80 parts, softens auxiliary agent
0.1~0.5 part, SBS be 3~5 parts, graphene is 2~3 parts, modified end dissaving polymer is 3~5 parts.Graphene adds
Enter the hydrophobicity that can increase material.
Further, in a preferred embodiment of the present invention, in parts by weight, reaction mixture is 90~100 parts, slides
Mountain flour is 2~3 parts, age resister is 0.1~0.4 part and toughener is 0.2~0.6 part.During the reaction be added talcum powder,
Age resister and toughener can effectively enhance modified asphalt waterproof coiled material anti-aging property.
Step S7: nonwoven layer tire base upper and lower surfaces are respectively coated into one layer of modified pitch and obtain modified asphalt layer, are being changed
Property pitch layer surface bond PE film, through cooling, meter is long, trimming and winds waterproof roll is made.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation methods of above-mentioned modified asphalt waterproof coiled material, comprising the following steps:
Step S1: use DMAC N,N' dimethyl acetamide by 133.19g diisopropanolamine (DIPA), 2.67gN- chlorosuccinimide (as drawing
Send out agent), 2g magnetic Fe3O4Microballoon dissolution, and it is settled to 1L, the concentration that diisopropanolamine (DIPA) is made is the diisopropanolamine (DIPA) of 1mol/L
Mixed solution.In the present embodiment, organic solvent is n,N-dimethylacetamide, and in other embodiments, organic solvent can be with
It is at least one of n,N-dimethylacetamide, dimethylformamide and cyclohexanone, the present embodiment can be realized as organic
The technical effect of solvent, all in the protection scope of the present embodiment.N- chlorosuccinimide is as initiator, in diisopropanol
It is added in amine course of dissolution, it can be in subsequent preparation AB2Play the role of causing polymerization during monomer mixed solution.If in AB2
During monomer synthesizes, magnetic Fe is added3O4Microballoon can play positive effect in subsequent microwave reaction, so that instead
The final product modified asphalt waterproof coiled material effect that should be obtained is more preferable.It is modification obtained when the ratio of above-mentioned substance is aforementioned proportion
Asphalt water-proof coiled material effect is the most excellent.
Step S2: being dissolved in n,N-dimethylacetamide and be settled to 1L for 288.18g trimellitic anhydride, and concentration is made
For the trimellitic acid anhydride solution of 1.5mol/L；
Step S3: it takes 100ml trimellitic acid anhydride solution as in there-necked flask, is under nitrogen atmosphere protection, and in ultrasound intensity
100ml diisopropanolamine (DIPA) mixed solution is added in 66ml trimellitic acid anhydride solution under conditions of 40Hz, and in the super of 50Hz
Under acoustic environment, AB is made after 6h is reacted at 35 DEG C2Monomer mixed solution；
Step S4: above-mentioned AB is taken2Monomer mixed solution 100ml, and 0.597g(0.004mol is added wherein) triethanolamine,
0.180g toluenesulfonic acid and 80ml toluene, prepared by microwave reaction dissaving polymer solution under the conditions of oil bath temperature is 140 DEG C,
Wherein, microwave intensity control is in 2300MHz；During preparing dissaving polymer, the triethanolamine of addition is as core point
Son, toluenesulfonic acid can effectively improve the conversion ratio of polymerization reaction as catalyst.Meanwhile band water being added during the reaction
Agent can timely take away moisture obtained in reaction process, accelerate the rate that reaction carries out.In many Practical in Chemistry,
Microwave reaction can generate more positive effect, thus the knowledge for the microwave chemical that has also been born to the final result of chemical reaction
System.It is found by creative work of the invention, it, can be effective in this step in the lower carry out polymerization reaction of microwave condition
Raising reaction conversion ratio.
Step S5: by 70ml dissaving polymer solution, 5.3g methyl acrylate and 0.1g toluenesulfonic acid mix and it is abundant
Dissolution, and bath temperature is that modified end dissaving polymer solution, warp is made in 88 DEG C of condensing reflux 5h reactions in there-necked flask
Modified end dissaving polymer is made after vacuum distillation；
Step S6: 20min is mixed to uniform in 75g bitumen base, 0.5g softening auxiliary agent, 3g is added in the above system
SBS, 3g graphene, the modified end dissaving polymer of 3g, 3h is reacted under the conditions of being placed on 170 DEG C after mixing, reaction is made
Mixture；Above-mentioned 45g reaction mixture, filler material 1.5g talcum powder are uniformly mixed, 0.05g age resister, 0.3g are added
Toughener is stirred to react 1h and modified pitch is made；
Step S7: the modified pitch that nonwoven layer tire base upper and lower surfaces respectively coat one layer of above-mentioned steps S6 preparation is changed
Property bitumen layer, bond PE film in above-mentioned modified pitch layer surface, through cooling, meter is long, trimming and winds waterproof roll is made.
Embodiment 2
The present embodiment provides a kind of preparation methods of above-mentioned modified asphalt waterproof coiled material, comprising the following steps:
Step S1: use dimethylformamide by 146.5g diisopropanolamine (DIPA), 1.34gN- chlorosuccinimide (as initiation
Agent), 1g magnetic Fe3O4Microballoon dissolution, and it is settled to 1L, the concentration that diisopropanolamine (DIPA) is made is the diisopropanolamine (DIPA) of 1.1mol/L
Mixed solution.In the present embodiment, organic solvent is dimethylformamide, and in other embodiments, organic solvent can be N,
At least one of N- dimethyl acetamide, dimethylformamide and cyclohexanone can realize the present embodiment as organic solvent
Technical effect, all in the protection scope of the present embodiment.N- chlorosuccinimide is molten in diisopropanolamine (DIPA) as initiator
It is added in solution preocess, it can be in subsequent preparation AB2Play the role of causing polymerization during monomer mixed solution.If in AB2Monomer
During synthesis, magnetic Fe is added3O4Microballoon can play positive effect in subsequent microwave reaction, so that reacting
The final product modified asphalt waterproof coiled material effect arrived is more preferable.It is modified pitch obtained when the ratio of above-mentioned substance is aforementioned proportion
Waterproof roll effect is the most excellent.
Step S2: 192.12g trimellitic anhydride is dissolved in dimethylformamide and is settled to 1L, obtained concentration is
The trimellitic acid anhydride solution of 1mol/L；
Step S3: it takes 100ml trimellitic acid anhydride solution as in there-necked flask, is under nitrogen atmosphere protection, and in ultrasound intensity
83ml diisopropanolamine (DIPA) mixed solution is added in 100ml trimellitic acid anhydride solution under conditions of 50Hz, and in the super of 50Hz
Under acoustic environment, AB is made after 4h is reacted at 45 DEG C2Monomer mixed solution；
Step S4: above-mentioned AB is taken2Monomer mixed solution 100ml, and 0.90g triethanolamine, 0.140g toluenesulfonic acid are added wherein
With 75ml benzene, prepared by microwave reaction dissaving polymer solution under the conditions of oil bath temperature is 145 DEG C, wherein microwave intensity control
System is in 2000MHz；During preparing dissaving polymer, the triethanolamine of addition is as core molecule, toluenesulfonic acid conduct
Catalyst can effectively improve the conversion ratio of polymerization reaction.Meanwhile during the reaction be added water entrainer can timely by
Moisture obtained in reaction process is taken away, and the rate that reaction carries out is accelerated.In many Practical in Chemistry, microwave reaction can be right
The final result of chemical reaction generates more positive effect, thus the knowledge hierarchy for the microwave chemical that has also been born.By this hair
Bright creative work discovery, in this step in the lower carry out polymerization reaction of microwave condition, can effectively improve reaction
Conversion ratio.
Step S5: by 80ml dissaving polymer solution, 5.0g methyl acrylate and 0.12g toluenesulfonic acid mix and it is abundant
Dissolution, and bath temperature is the obtained modified end dissaving polymer solution of 92 DEG C of condensing reflux 7h reactions in there-necked flask, then
Modified end dissaving polymer is being made after being evaporated under reduced pressure；
Step S6: 40min is mixed to uniform in 80g bitumen base, 0.1g softening auxiliary agent, 5g is added in the above system
SBS, 2g graphene, the modified end dissaving polymer of 5g, 1h is reacted under the conditions of being placed on 185 DEG C after mixing, reaction is made
Mixture；Above-mentioned 50g reaction mixture, 1 g talcum powder of filler material are uniformly mixed, add 0.2g age resister, 0.1g increases
Tough dose is stirred to react 2h and modified pitch is made；
Step S7: the modified pitch that nonwoven layer tire base upper and lower surfaces respectively coat one layer of above-mentioned steps S6 preparation is changed
Property bitumen layer, bond PE film in above-mentioned modified pitch layer surface, through cooling, meter is long, trimming and winds waterproof roll is made.
Embodiment 3
The present embodiment provides a kind of preparation methods of above-mentioned modified asphalt waterproof coiled material, comprising the following steps:
Step S1: use cyclohexanone that 199.8g diisopropanolamine (DIPA), 4gN- chlorosuccinimide (as initiator), 2g is magnetic
Fe3O4Microballoon dissolution, and it is settled to 1L, the concentration that diisopropanolamine (DIPA) is made is the diisopropanolamine (DIPA) mixed solution of 1.5mol/L.?
In the present embodiment, organic solvent is cyclohexanone, and in other embodiments, organic solvent can be n,N-dimethylacetamide, two
At least one of methylformamide and cyclohexanone can realize technical effect of the present embodiment as organic solvent, all at this
In the protection scope of embodiment.N- chlorosuccinimide is added in diisopropanolamine (DIPA) course of dissolution as initiator, can
In subsequent preparation AB2Play the role of causing polymerization during monomer mixed solution.If in AB2During monomer synthesizes, it is added
Magnetic Fe3O4Microballoon can play positive effect in subsequent microwave reaction, so that the final product modified pitch that reaction obtains
Waterproof roll effect is more preferable.It is that modified asphalt waterproof coiled material effect obtained is the most excellent when the ratio of above-mentioned substance is aforementioned proportion
It is different.
Step S2: 192.12g trimellitic anhydride is dissolved in dimethylformamide and is settled to 1L, obtained concentration is
The trimellitic acid anhydride solution of 1mol/L；
Step S3: it takes 165ml trimellitic acid anhydride solution as in there-necked flask, is under nitrogen atmosphere protection, and in ultrasound intensity
100ml diisopropanolamine (DIPA) mixed solution is added in 165ml trimellitic acid anhydride solution under conditions of 45Hz, and in the super of 45Hz
Under acoustic environment, AB is made after anti-5h at 40 DEG C2Monomer mixed solution；
Step S4: above-mentioned AB is taken2Monomer mixed solution 100ml, and 0.75g triethanolamine, 0.160g toluenesulfonic acid are added wherein
With 78ml benzene, prepared by microwave reaction dissaving polymer solution under the conditions of oil bath temperature is 142 DEG C, wherein microwave intensity control
System is in 2000MHz；During preparing dissaving polymer, the triethanolamine of addition is as core molecule, toluenesulfonic acid conduct
Catalyst can effectively improve the conversion ratio of polymerization reaction.Meanwhile during the reaction be added water entrainer can timely by
Moisture obtained in reaction process is taken away, and the rate that reaction carries out is accelerated.In many Practical in Chemistry, microwave reaction can be right
The final result of chemical reaction generates more positive effect, thus the knowledge hierarchy for the microwave chemical that has also been born.By this hair
Bright creative work discovery, in this step in the lower carry out polymerization reaction of microwave condition, can effectively improve reaction
Conversion ratio.
Step S5: by 75ml dissaving polymer solution, 5.1g methyl acrylate and 0.1g toluenesulfonic acid mix and it is abundant
Dissolution, and the water bath condition in there-necked flask, temperature are that the obtained modified end dissaving polymer of 88 DEG C of condensing reflux 5h reactions is molten
Modified end dissaving polymer is made in liquid after being evaporated under reduced pressure；
Step S6: 30min is mixed to uniform in 80g bitumen base, 0.3g softening auxiliary agent, is added 4g's in the above system
The modified end dissaving polymer of SBS, 2g graphene, 4g reacts 2h and is made and reacts mixed under the conditions of being placed on 180 DEG C after mixing
Close object；Above-mentioned 47.5g reaction mixture, 1 g talcum powder of filler material are uniformly mixed, add 0.1g age resister, 0.2g increases
Tough dose is stirred to react 2h and modified pitch is made；
Step S7: the modified pitch that nonwoven layer tire base upper and lower surfaces respectively coat one layer of above-mentioned steps S6 preparation is changed
Property bitumen layer, bond PE film in above-mentioned modified pitch layer surface, through cooling, meter is long, trimming and winds waterproof roll is made.
Embodiment 4
The present embodiment provides a kind of preparation methods of above-mentioned modified asphalt waterproof coiled material, comprising the following steps:
Step S1: use DMAC N,N' dimethyl acetamide by 166.49g diisopropanolamine (DIPA), 2.5gN- chlorosuccinimide (as drawing
Send out agent), 1.875g magnetic Fe3O4Microballoon dissolution, and is settled to 1L, and the concentration that diisopropanolamine (DIPA) is made is the two different of 1.25mol/L
Propanolamine mixed solution.In the present embodiment, organic solvent is n,N-dimethylacetamide, in other embodiments, You Jirong
Agent can be at least one of n,N-dimethylacetamide, dimethylformamide and cyclohexanone, can realize that the present embodiment is made
For the technical effect of organic solvent, all in the protection scope of the present embodiment.N- chlorosuccinimide is as initiator, two
It is added in isopropanolamine course of dissolution, it can be in subsequent preparation AB2Play the role of causing polymerization during monomer mixed solution.
If in AB2During monomer synthesizes, magnetic Fe is added3O4Microballoon can play positive effect in subsequent microwave reaction,
So that the final product modified asphalt waterproof coiled material effect that reaction obtains is more preferable.It is obtained when the ratio of above-mentioned substance is aforementioned proportion
Modified asphalt waterproof coiled material effect it is the most excellent.
Step S2: 240.15g trimellitic anhydride is dissolved in dimethylformamide and is settled to 1L, obtained concentration is
The trimellitic acid anhydride solution of 1.25mol/L；
Step S3: it takes 105ml trimellitic acid anhydride solution as in there-necked flask, is under nitrogen atmosphere protection, and in ultrasound intensity
100ml diisopropanolamine (DIPA) mixed solution is added in 105ml trimellitic acid anhydride solution under conditions of 45Hz, and in the super of 45Hz
Under acoustic environment, AB is made after anti-5h at 40 DEG C2Monomer mixed solution；
Step S4: above-mentioned AB is taken2Monomer mixed solution 100ml, and 0.746g triethanolamine, 0.160g toluenesulfonic acid are added wherein
With 77ml benzene, prepared by microwave reaction dissaving polymer solution under the conditions of oil bath temperature is 143 DEG C, wherein microwave intensity control
System is in 2150MHz；During preparing dissaving polymer, the triethanolamine of addition is as core molecule, toluenesulfonic acid conduct
Catalyst can effectively improve the conversion ratio of polymerization reaction.Meanwhile during the reaction be added water entrainer can timely by
Moisture obtained in reaction process is taken away, and the rate that reaction carries out is accelerated.In many Practical in Chemistry, microwave reaction can be right
The final result of chemical reaction generates more positive effect, thus the knowledge hierarchy for the microwave chemical that has also been born.By this hair
Bright creative work discovery, in this step in the lower carry out polymerization reaction of microwave condition, can effectively improve reaction
Conversion ratio.
Step S5: 75ml dissaving polymer solution, 5.15g methyl acrylate and 0.11g toluenesulfonic acid are mixed and is filled
Divide dissolution, and the water bath condition in there-necked flask, temperature, which is that 90 DEG C of condensing reflux 6h reactions are obtained, is modified end dissaving polymer
Modified end dissaving polymer is made in solution after being evaporated under reduced pressure；
Step S6: 30min is mixed to uniform in 78g bitumen base, 0.2g softening auxiliary agent, is added 4g's in the above system
The modified end dissaving polymer of SBS, 2.5g graphene, 4g reacts 2h and reaction is made under the conditions of being placed on 177 DEG C after mixing
Mixture；Above-mentioned 47.5g reaction mixture, 1.25 g talcum powder of filler material are uniformly mixed, add 0.15g age resister,
0.2g toughener is stirred to react 1h and modified pitch is made；
Step S7: the modified pitch that nonwoven layer tire base upper and lower surfaces respectively coat one layer of above-mentioned steps S6 preparation is changed
Property bitumen layer, bond PE film in above-mentioned modified pitch layer surface, through cooling, meter is long, trimming and winds waterproof roll is made.
Comparative example 1
The present embodiment provides a kind of preparation method of modified asphalt waterproof coiled material, modified asphalt waterproof coiled material provided in this embodiment
Preparation method and embodiment 4 provide modified asphalt waterproof coiled material preparation method the difference is that: in step S4 system
Microwave is not added during standby dissaving polymer solution.
Comparative example 2
The present embodiment provides a kind of preparation method of modified asphalt waterproof coiled material, modified asphalt waterproof coiled material provided in this embodiment
Preparation method and embodiment 4 provide modified asphalt waterproof coiled material preparation method the difference is that: in step S6 system
Graphene is not added during standby modified pitch.
Comparative example 3
The present embodiment provides a kind of preparation method of modified asphalt waterproof coiled material, modified asphalt waterproof coiled material provided in this embodiment
Preparation method and embodiment 4 provide modified asphalt waterproof coiled material preparation method the difference is that: it is molten in step S1
Magnetic Fe is not added during solution diisopropanolamine (DIPA) 3O 4Microballoon.
The detection of 1 modified asphalt waterproof coiled material of test example
Modified asphalt waterproof made from Examples 1 to 4 and comparative example 1~3 is rolled up and is examined according to GB/T23457-2009 standard
It surveys, and result is included in table 1.
Table 1: the performance test results of the modified asphalt waterproof coiled material of Examples 1 to 4 and comparative example 1~3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Transverse tensile strength Mpa | 32.3 | 32.8 | 31.7 | 28.3 | 41.3 | 36.1 | 35.2 |
| Transverse breakage elongation % | 683 | 679 | 684 | 621 | 767 | 721 | 715 |
| Longitudinal tensile strength Mpa | 38.9 | 39.5 | 40.2 | 35.8 | 47.3 | 43.5 | 42.9 |
| Longitudinal elongation at break rate % | 611 | 622 | 617 | 568 | 673 | 647 | 647 |
| Cross-breaking strength N/mm | 73 | 75 | 73 | 67 | 92 | 86 | 84 |
| Longitudinal fracture intensity N/mm | 30 | 32 | 30 | 24 | 37 | 35 | 34 |
| High temperature resistant DEG C | 52 | 52 | 51 | 54 | 49 | 51 | 50 |
| Low temperature resistant DEG C | -37 | -37 | -36 | -40 | -33 | -35 | -35 |
By testing result in table 1 it is found that Examples 1 to 4 is made using the preparation method of modified asphalt waterproof coiled material of the invention
Modified asphalt waterproof coiled material it is preferable as a result, explanation exists compared to all having with comparative example 1~3 in terms of mechanical property and heatproof
The reaction for preparing dissaving polymer solution is no plus microwave, during preparing pitch plus graphene, in configuration diisopropyl
Add magnetic Fe during hydramine mixed solution3O4Microballoon all generates certain product to last modified asphalt waterproof coiled material performance
Pole influences.Also, modified asphalt waterproof made from the comparative example 1 of microwave is not added in the reaction for preparing dissaving polymer solution
Coiled material either mechanical property or heat resistance is all worse, illustrates the importance for adding microwave during the reaction.
In conclusion dissaving polymer is first prepared the present invention relates to a kind of preparation method of modified asphalt waterproof coiled material,
It recycles above-mentioned dissaving polymer with SBS together modified synergic pitch, finally prepares modified asphalt waterproof coiled material.On firstly,
The preparation method of modified asphalt waterproof coiled material is stated compared with the independent modified pitch of traditional SBS, because controlling costly
The dosage of SBS, so cost is lower.Secondly, dissaving polymer can be good at being directly dissolved in pitch at a lower temperature,
So that the pitch of synthesis has preferable performance.Again, do not needed in the manufacturing process of waterproof roll as SBS through it is too long when
Between high temperature grinding, preparation process is simpler.Finally, joined magnetic Fe in the raw material of reaction 3O 4Microballoon simultaneously passes through micro-
The modified asphalt waterproof coiled material that wave reaction is prepared is had excellent performance.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of modified asphalt waterproof coiled material, which comprises the steps of:
Step S1: by diisopropanolamine (DIPA), initiator, magnetic Fe3O4Microballoon and organic solvent are mixed to prepare the diisopropanolamine (DIPA)
Concentration is the diisopropanolamine (DIPA) mixed solution of 1~1.5mol/L, and the organic solvent is n,N-dimethylacetamide, dimethyl methyl
At least one of amide and cyclohexanone；
Step S2: trimellitic anhydride is dissolved in the organic solvent, and the trimellitic anhydride that concentration is 1~1.5mol/L is made
Solution；
Step S3: the diisopropanolamine (DIPA) mixed solution is added to the trimellitic acid anhydride solution under inert gas protection
In, and react 4~6h under the conditions of 35~45 DEG C under ultrasound condition and AB is made2Monomer mixed solution；
Step S4: in the AB2Triethanolamine, toluenesulfonic acid and water entrainer are added in monomer mixed solution, in 140~145 DEG C of temperature
Prepared by microwave reaction dissaving polymer solution in range；
Step S5: by the dissaving polymer solution, methyl acrylate and toluenesulfonic acid mix after temperature be 88~92 DEG C
It is condensed back 5~7h reaction and modified end dissaving polymer solution is made, it is hyperbranched that modified end is made after being evaporated under reduced pressure
Polymer；
Step S6: after 20~40min is mixed in bitumen base, softening auxiliary agent, addition SBS, graphene, modified end are super
Branched polymer reacts 1~3h under the conditions of 170~185 DEG C and reaction mixture is made；The reaction mixture, talcum powder are mixed
It closes uniformly, adds age resister, toughener is stirred to react 1~2h and modified pitch is made；
Step S7: nonwoven layer tire base upper and lower surfaces are respectively coated into one layer of modified pitch and obtain modified asphalt layer, are changed described
Property pitch layer surface bond PE film, through cooling, meter is long, trimming and winds waterproof roll is made.
2. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S3
The intensity of ultrasonic treatment is 40~50Hz.
3. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S3
The amount ratio of diisopropanolamine (DIPA) in diisopropanol amine aqueous solution and the trimellitic anhydride in the trimellitic acid anhydride solution is 1mol:
1~1.1mol.
4. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S4
Water entrainer is one of toluene or benzene.
5. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S4
AB2Monomer mixed solution, the triethanolamine, the toluenesulfonic acid and the water entrainer amount ratio be 100ml:0.004~
0.006mol:0.140~0.180g:75~80ml.
6. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S4
The microwave intensity of microwave reaction is 2000~2300MHz.
7. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S1
Diisopropanolamine (DIPA), the initiator and the magnetic Fe3O4The amount ratio of microballoon be 0.100~0.110mol:0.001~
0.002mol:0.1~0.2g.
8. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that described in step S5
The amount ratio of dissaving polymer solution, the methyl acrylate and the toluenesulfonic acid be 70~80ml:5~5.3g:0.1~
0.12g。
9. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that in step S6, according to
Parts by weight meter, the bitumen base is 75~80 parts, 0.1~0.5 part of auxiliary agent of softening, SBS are 3~5 parts, graphene is 2~3
Part, modified end dissaving polymer are 3~5 parts.
10. the preparation method of modified asphalt waterproof coiled material according to claim 1, which is characterized in that in step S6, according to
Parts by weight meter, the reaction mixture is 90~100 parts, talcum powder is 2~3 parts, age resister is 0.1~0.4 part and is increased
Tough dose is 0.2~0.6 part.
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