CN114395370A - Sizing material for improving stripping performance and construction applicability of S-CLF YC type coiled material - Google Patents

Sizing material for improving stripping performance and construction applicability of S-CLF YC type coiled material Download PDF

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CN114395370A
CN114395370A CN202111653854.6A CN202111653854A CN114395370A CN 114395370 A CN114395370 A CN 114395370A CN 202111653854 A CN202111653854 A CN 202111653854A CN 114395370 A CN114395370 A CN 114395370A
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rubber
asphalt
lignin
coiled material
stirring
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吴帅
王聪迪
曹进明
缪线生
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Suzhou Zhuobao Tech Co ltd
Shenzhen Zhuobao Technology Co Ltd
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Suzhou Zhuobao Tech Co ltd
Shenzhen Zhuobao Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J195/00Adhesives based on bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a sizing material for improving the stripping performance and construction applicability of an S-CLF YC type coiled material, which can overcome the defect that the stripping strength of the coiled material and post-cast concrete is not satisfactory when asphalt, an oil product, SBS, butyl rubber, SBR, lignin, tackifying resin and stone powder are compounded in a specific range, and can level the appearance of the S-CLF YC type waterproof coiled material, so that the phenomena of sand surface and yellowing of the coiled material are not easily caused under a high-temperature condition, and the other performances are ensured to meet the requirements of standards. The performance of the coiled material is improved, and the market competitiveness of the product is improved.

Description

Sizing material for improving stripping performance and construction applicability of S-CLF YC type coiled material
Technical Field
The invention belongs to the technical field of building material production, and particularly relates to a sizing material for improving the stripping performance and construction applicability of an S-CLF YC type coiled material. The invention also relates to a method for producing said rubber compounds.
Background
The waterproof coiled material is developed very rapidly since the 80 th of the 20 th century, has the advantages of light weight, high tensile strength, high elongation, good weather resistance, large use temperature range, small pollution and the like, gradually becomes one of very common building materials for modern buildings, is mainly used for building walls, roofs, tunnels, highways, landfill sites and other places at present, can play a role in resisting external rainwater and groundwater leakage, is used as a leakage-free connection between an engineering foundation and a building, is a first barrier for waterproofing of the whole engineering, and plays a vital role in the whole engineering. The waterproof roll is mainly divided into an asphalt waterproof roll and a high-molecular waterproof roll, wherein a strong cross laminated film self-adhesive waterproof roll (S-CLF waterproof roll) researched and developed in the current market can integrate the advantages of the high-molecular roll and a self-adhesive modified asphalt waterproof roll and avoid respective defects, the physical property is excellent, and the tensile property is 2-3 times of that of the traditional tubeless self-adhesive roll. The waterproof paint is light, thin and soft, the thickness is less than or equal to 2mm, the construction is convenient, the tearing strength is high, and the waterproof effect is good.
The S-CLF waterproof coiled material is formed by combining an imported super-strong cross laminated film, a self-adhesive rubber asphalt sizing material with a high-performance formula and an isolating film, is a tubeless self-adhesive waterproof coiled material with very good tensile, elongation and tear resistance, and has excellent ultraviolet resistance and stability. The S-CLF waterproof roll mainly comprises three types, namely single-sided self-adhesion (NS type), double-sided self-adhesion (ND type) and pre-laid reverse adhesion (YC type), wherein the single-sided self-adhesion (NS type) consists of a strong cross laminated film, self-adhesion rubber asphalt sizing material and a separating film; the double-sided self-adhesive (ND type) is composed of an aluminized isolating film, a self-adhesive rubber asphalt sizing material, a strong cross laminated film, a self-adhesive rubber asphalt sizing material and an isolating film; the pre-laid reverse adhesion (YC type) is composed of an anti-adhesion and anti-adhesion layer, a self-adhesive rubber asphalt sizing material, a strong cross laminated film, a self-adhesive rubber asphalt sizing material and an isolating film. Particularly, the S-CLF YC type waterproof coiled material is a double-sided self-adhesive pre-paved waterproof coiled material, and the upper surface of the S-CLF YC type waterproof coiled material is an anti-sticking and anti-sticking layer, so that the problems of ultraviolet irradiation and sticking of feet in the binding process of reinforcing steel bars can be effectively prevented; when the basement bottom plate is constructed, the waterproof material can be reversely bonded with post-cast concrete, so that the skin type waterproof effect is realized, and the waterproof material becomes a new favorite of the existing building materials.
However, the existing S-CLF YC type waterproof coiled material generally has the defects of poor appearance and easy shedding of colored sand coated on the surface, and under the condition of high temperature in summer, the part remained on the surface of the coiled material is easy to sink after the colored sand coated on the surface of the S-CLF YC type waterproof coiled material is shed, and oil in asphalt sizing material is separated out, so that the defects of sand surface and yellowing of the surface of the coiled material are easily caused. In addition. The peel strength of the existing S-CLF YC type waterproof coiled material and post-cast concrete does not meet the parameter requirement in the enterprise standard Q/320584PAI011-2019, and the viscosity of the rubber material is large during modification, which is not beneficial to stirring, and the dissolution degree of the modifier cannot reach the best. Therefore, how to improve the construction applicability and the peeling performance of the S-CLF YC type waterproof roll becomes one of the research targets of researchers and producers in the industry.
CN 112662374B discloses a sizing material for improving the stripping performance of S-CLF coiled materials by an acid-base regulator, which comprises the following raw materials in percentage by weight: 40-60% of asphalt, 4-9% of modified oil, 4-9% of SBS, 2-8% of pre-sol, 0.5-1.5% of SBR, 0.03-0.08% of heat stabilizer, 0.03-0.08% of modified petroleum resin, 4-10% of acid-base regulator and the balance of filling powder. The rubber material uses SBS, pre-sol and SBR in cooperation with modified oil and asphalt, so that rubber, asphalt and modified oil are better combined, the adhesion effect of the rubber waterproof coating relative to a base layer is improved, and the waterproof effect is enhanced. CN 112680184B discloses a rubber material with a curing agent for improving the stripping performance of S-CLF coiled materials, which comprises the following raw materials in percentage by weight: 40-60% of asphalt, 4-9% of modified oil, 4-9% of SBS, 2-8% of pre-sol, 0.5-1.5% of SBR, 0.01-0.08% of heat stabilizer, 0.01-0.08% of modified petroleum resin, 1-8% of curing agent and the balance of filling powder. The sizing material optimizes the formula of the sizing material, achieves the purposes of reducing the viscosity of the sizing material and improving the performance of the sizing material through component selection and content proportion, has excellent stripping performance through combination and compounding of the components, solves the problem that the stripping strength of an S-CLF sizing material coiled material and post-cast concrete has defects, and simultaneously ensures that other performances meet the requirements of standards. However, the curing agent and the acid-base regulator in the two sizing materials have strict requirements on storage environment and conditions, are easy to react with water and oxygen in the air, and cannot achieve the original effect, and the sizing material has improved stripping performance, but is not improved in the aspect of construction applicability of S-CLF type coiled materials.
In summary, it is urgent to provide a sizing material for S-CLF YC waterproof rolls so that the S-CLF YC waterproof rolls have good peeling performance and improved construction applicability.
Disclosure of Invention
In order to solve the problems, the invention researches the composition and construction process of the existing waterproof coiled material, and finds that the rubber material obtained when asphalt, oil, SBS, butyl rubber, SBR, lignin, tackifying resin and stone powder are compounded in a specific range can improve the defect that the peeling strength of the coiled material and post-cast concrete is not satisfactory, and the S-CLF YC type waterproof coiled material has smooth appearance, is not easy to cause the phenomena of sand surface and yellowing of the coiled material under the high-temperature condition, and simultaneously ensures that other performances meet the standard requirements. The performance of the coiled material is improved, and the market competitiveness of the product is improved.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a sizing material for improving the stripping performance and construction applicability of an S-CLF YC type coiled material comprises the following components in parts by weight:
Figure BDA0003447731250000031
through a great deal of research, the existing glue stock of the S-CLF type waterproof roll has a great deal of free oil content, and the phenomenon of precipitation is easy to occur under the high-temperature condition of summer. In addition, the whole rubber material is soft and has high penetration, so that colored sand coated on the surface is easy to sink into the rubber material to cause local blackening of the coiled material, and meanwhile, the viscosity of the rubber material is insufficient, so that the adhesive force to the colored sand is insufficient, and the colored sand is easy to fall off. The invention optimizes the formula of the sizing material, improves the performance of the sizing material through component selection and content proportion, solves the problem that the peeling strength of the S-CLFYC type coiled material and post-cast concrete has defects, improves the appearance of the coiled material and ensures that other performances meet the requirements of standards. Through a large amount of experimental researches, the inventor selects and compounds a plurality of raw materials, particularly properly uses lignin and butyl rubber, and can fully absorb the free oil content in the rubber material, so that the oil content can not be separated out from the coiled material under high temperature conditions such as summer and the like, and the phenomena of yellowing and blackening are avoided; meanwhile, lignin can increase the adhesiveness of the rubber material, mineral aggregate, concrete, cement mortar and the like, so that the adsorption force of the waterproof coiled material on the colored sand coated on the surface is increased, the waterproof coiled material is not easy to fall off, and meanwhile, the stripping performance of the S-CLF coiled material and post-cast concrete is good, and the parameter requirements in the enterprise mark Q/320584PAI011-2019 are met.
It is particularly noted that, in the invention, the purpose of the invention is achieved by the combination and compounding of the components, specifically, the oil compatibilizes the main components of asphalt, SBS, lignin, butyl rubber and SBR in the rubber compound, so that the components are uniformly dispersed; the SBS is adopted to improve the toughness and high and low temperature resistance of the asphalt and increase the elasticity; the cohesion and the bonding force of the rubber compound are increased by mutually matching butyl rubber, SBR and lignin; the penetration degree of the rubber material is reduced and the adhesiveness is increased through the tackifying resin. The content of all the components is set, so that the viscosity of the rubber material is improved, the flowing of asphalt is prevented, the cohesiveness of the rubber material is increased, the problem that the surface-coated colored sand is easy to fall off is solved, the stripping performance of the S-CLF YC type waterproof coiled material and post-cast concrete is good, and the parameter requirement in the enterprise label Q/320584PAI011-2019 is met.
In addition, in the present invention, additives conventionally used in the art may be added according to actual use needs and the addition amount may be adjusted empirically, such as one or more of surfactants, thickeners, toughening agents, pigments, and the specific kind and amount thereof may be self-weighed by those skilled in the art according to actual needs, and the present invention is not particularly limited thereto.
Preferably, in the above-mentioned compound, the asphalt is common road asphalt, more preferably road petroleum asphalt with a grade of 70-110, such as one or more of 70# petroleum asphalt, 90# petroleum asphalt, 100# petroleum asphalt, 110# petroleum asphalt, 130# petroleum asphalt, 140# petroleum asphalt, etc.
Further preferably, in the above-mentioned compound, the asphalt is one or more of 90# asphalt, 100# asphalt, and 110# asphalt, and most preferably 90# asphalt, and particularly preferably 90# asphalt obtained from the companies of the china petroleum chemical industry group, the china petroleum and natural gas group, and/or the korean SK group. Wherein the index of the 90# asphalt is 80-100; the 15-degree ductility AB grade is greater than 100, and the C grade is greater than 50; softening points 1-2 and 1-3 and 1-4 zones have a class A greater than 45, a class B greater than 43, a class C greater than 42, a class 2-2 and 2-3 class A greater than 44, a class B greater than 42, and a class C greater than 42.
The asphalt is used as a main material of the sizing material, and needs to have very good hydrophobicity, which is a basic guarantee for the impermeability of the waterproof roll; meanwhile, the asphalt material also needs to have a certain softening point and penetration degree, wherein the softening point of the asphalt refers to a condition viscosity in a range from solid state to liquid state transition temperature of the artificially selected asphalt and is also the temperature when the asphalt reaches the specified condition viscosity, and the softening point of the asphalt is an important index for reflecting the temperature stability of the asphalt material; the penetration degree represents the softness and hardness degree and the consistency of the asphalt and the ability of shearing and shearing resistance, reflects the index of relative viscosity under certain conditions, and is a main reference index for asphalt grading. Through a large number of experiments and researches on various asphalts, the inventor of the invention finds that 90# petroleum asphalt, particularly 90# petroleum asphalt, is used as an asphalt material, and the coating obtained by the rubber material has the best appearance and excellent physical and mechanical properties. It can be seen that the choice of the bituminous host material is also very important.
Preferably, in the above rubber compound, the oil is a heavy aromatic oil having a viscosity of 5000mpa.s or less and an aniline point of 45 ℃ or less. Viscosity and aniline point are the main quality indexes for characterizing the composition and physical properties of aromatic oil, wherein the low-viscosity aromatic oil can enable vulcanized rubber to have lower hardness and low-temperature elasticity, and the lower the aniline point is, the higher the aromatic content is, the better the compatibility with rubber is; therefore, the invention needs to select oil products with low viscosity and low aniline point, particularly oil products with viscosity below 5000mpa.s and amine point below 45 ℃, such as 60# oil product purchased from Shenzhen treasure Shenpetrochemical company and 35# oil product purchased from Anhui eastern Jiaxin building materials science and technology company, both of which can improve the high and low temperature performance and the thermal aging performance of the rubber compound, improve the melting degree of other raw materials, and can compatibilize main components such as asphalt, SBS, lignin, butyl rubber and SBR in the rubber compound so that all components are uniformly dispersed. In other words, the oil product serves as a base oil to improve the low-temperature performance of the rubber compound of the invention, and simultaneously serves as a solvent, and the addition of the oil product adjusts the asphalt to proper fluidity and can improve the dissolution degree of other raw material components, so that the rubber compound of the invention is more homogenized, and the stability of the performance is facilitated.
It should be noted that the heavy aromatic hydrocarbon refers to an aromatic hydrocarbon of above C10, and at present, C8 and C9 are listed therein, and the main component is an aromatic hydrocarbon with a benzene ring structure. The kind and source of the heavy aromatic oil are not particularly limited, and those recognized by those skilled in the art can be used.
Preferably, in the above rubber compound, the weight ratio of the asphalt to the oil is (3-6): 1. the weight ratio of bitumen to oil in this range enables the components of the compound to be adequately dispersed and dissolved.
Preferably, in the above compound, the SBS has a number average molecular weight of 25 to 35 ten thousand daltons and the weight percentage of the styrene block to the total weight of said SBS is 25 to 45%. SBS (styrene-butadiene-styrene triblock copolymer) is thermoplastic styrene-butadiene rubber, has the characteristics of plastics and rubber, and can improve the low-temperature flexibility and heat resistance of the rubber material, so that the rubber material has certain cohesive strength and elasticity.
Preferably, among the above compounds, SBS is polymerized by methods well known in the art and is also commercially available, such as 3411 and/or 3501 from Qiyang industries, Inc., Huizhou.
Preferably, in the above non-curable asphalt coating, the butyl rubber is composed of styrene-butadiene rubber, softening oil, SBS, wax powder and filler.
Further preferably, the butyl rubber is composed of 1502 styrene-butadiene rubber, aromatic oil, SBS, wax powder and talc powder. The 1502 styrene-butadiene rubber is non-pollution soft emulsion styrene-butadiene rubber, the polymerization degree is high, the performance is high, the aromatic oil is heavy aromatic oil, the heavy aromatic oil refers to aromatic hydrocarbon above C10, and C8 and C9 are also listed in the aromatic hydrocarbon. The heavy aromatic oil is generally called as heavy aromatic oil, the application commodity of which is 100# to 200# solvent oil, and the main component of the heavy aromatic oil is aromatic hydrocarbon with a benzene ring structure. The kind and source of the heavy aromatic oil of the present invention are not particularly limited, and those approved by those skilled in the art can be used. The SBS has no limitation on types, can be in a star shape or a linear shape, and greatly improves the performance of butyl rubber. The wax powder is one of polyethylene wax, polypropylene wax and polyamide wax, the type of the wax powder is not particularly limited, and the high-temperature performance is enhanced. The mesh number of the talcum powder is 150-250 meshes, the cost of the talcum powder under the particle size is moderate, the talcum powder is used as a filler, and the talcum powder is economic and does not influence the performance of the butyl rubber. In addition, the wax powder includes, but is not limited to, one or more of polyethylene wax powder, oxidized polyethylene wax powder, polypropylene wax powder, polyamide wax powder, and the like. More specifically, the type of the wax powder is not strictly limited, but the melting point thereof needs to be between 130-160 ℃, and the addition of the wax powder with the melting point in the range can significantly improve the high-temperature performance, thereby avoiding the phenomenon that the performance is deteriorated due to high temperature in actual use.
Further preferably, the wax powder may be commercially available, such as available from champion 602, manufactured by champion successful plastics materials ltd, which is a polyamide wax powder capable of significantly improving extensibility and heat resistance; 8903 produced by Shenzhen Luqi materials science and technology Limited is oxidized polyethylene wax powder, and can also improve the heat resistance.
It should be noted that the above wax powder is provided by way of example only, and actually, the SBS and wax powder used in butyl rubber do not need to be specifically provided, and are only conventional in the art.
Particularly preferably, the butyl rubber consists of the following components in percentage by weight:
Figure BDA0003447731250000061
the weight percentages of the components are based on the total weight of the butyl rubber.
More preferably, the preparation process of the butyl rubber comprises the steps of heating aromatic oil to 150-165 ℃, adding 1502 styrene butadiene rubber and SBS, controlling the system temperature at 170-185 ℃, stirring for 2.5-5h, adding wax powder, stirring for 0.5-1h, grinding until no particles exist, adding talcum powder, stirring uniformly, cooling and cooling to obtain the butyl rubber.
During the preparation of the butyl rubber, milling was required to render the mixed system particle free as determined by visual inspection of a sample taken after milling.
The butyl rubber is used for primarily modifying 1502 styrene-butadiene rubber, and compared with the condition that the styrene-butadiene rubber is added independently, the butyl rubber has excellent dispersibility, the initial adhesion and the permanent adhesion of the asphalt rubber are increased, and the stripping performance of the rubber is improved. In addition, the butyl rubber can endow S-CLF YC products with excellent low-temperature flexibility and stripping performance, which is unexpected compared with the addition of the components separately; meanwhile, the addition of the butyl rubber can shorten the production time of the asphalt rubber material, reduce the production energy consumption and improve the quality of the asphalt rubber material.
Further preferably, in the rubber compound, the weight portion of the butyl rubber is 2-3, the cost of the butyl rubber is somewhat high, and in order not to affect the cost of the whole rubber compound, the addition amount of the butyl rubber needs to be strictly controlled, so that the rubber compound is not high in cost and is not beneficial to wide application.
In the invention, as the butyl rubber contains SBR (styrene butadiene rubber), additional addition of SBR (styrene butadiene rubber) can be not needed, but the addition amount of SBR is possibly insufficient due to the fact that the amount of the butyl rubber is limited due to the requirement of cost, and the SBR is preferably added in an amount of 1-3 parts by weight, so that the cohesion and the cohesive force of rubber can be increased, the low-temperature performance of asphalt is improved, the softening point is improved, and the defects of S-CLF YC type waterproof coiled materials in the prior art can be overcome.
Preferably, in the above-mentioned compounds, the SBR may be polymerized by methods well known in the art, or may be commercially available, for example, 92% SBR manufactured by trades ltd, high, shandong.
Preferably, in the above-mentioned gum, the lignin may be modified lignin such as sulfonated lignin and phenolated lignin, or may be unmodified lignin.
The lignin fiber mainly consists of C, H, O elements, the microstructure of the lignin fiber is banded and bent, uneven and porous, the cross part is flat, and the lignin fiber has good toughness, dispersibility and chemical stability; the reinforcing agent is dispersed in a three-dimensional form in the asphalt mixture, and can play a role in reinforcing; meanwhile, the internal free oil content can be fully absorbed in the asphalt mixture, so that the produced rubber material has no oil content to overflow under the high-temperature condition, and the yellowing and blackening phenomena are avoided; meanwhile, after the lignin is added into the asphalt, the flow of the asphalt is prevented, the holding power to the asphalt is very strong, and the high-temperature resistance of the rubber material is also improved. More important is the binding of lignin: the lignin fiber can increase the adhesion of asphalt sizing material and mineral aggregate, and improve the adhesion between aggregates (such as cement or colored sand) or plates (such as aluminum plates) through the adhesion of an oil film (asphalt can only generate adhesion effect on other coarse and fine aggregates after a film is formed); the viscosity of the asphalt rubber added with the lignin is increased, the adsorption force on the colored sand is larger, and the asphalt rubber is not easy to fall off.
Preferably, in the above rubber compound, the tackifying resin is one or a mixture of two or more of coumarone resin, terpene resin, rosin resin, petroleum resin, phenol resin epoxy resin and xylene formaldehyde resin. Of course, the tackifying resin may be other types of tackifying resins known in the art.
Preferably, in the above sizing material, the weight ratio of the tackifying resin to the lignin is 1: (1-3), if too much tackifying resin is added to the compound of the invention, the softening point of the compound of the invention increases and the penetration decreases, the low temperature performance will be particularly poor, while if too much lignin is added, the viscosity of the compound will be too high to be productive.
The lignin and the tackifying resin are added simultaneously, so that the adhesive force and the cohesive force of the rubber compound can be obviously improved, and the existing problems of S-CLF YC products are solved in a targeted manner.
Preferably, in the rubber compound, the filler is one or more of talcum powder, fly ash, heavy calcium carbonate and light calcium carbonate. The use of the filler can reduce the cost of the whole rubber compound, so that the cost of a user is reduced, the large-scale application of the rubber compound is facilitated, and the hardness of the rubber compound can be adjusted by using the filler.
Preferably, in the rubber compound, the filler has a particle size of less than 250 meshes, more preferably between 150 meshes and 200 meshes, the larger the mesh number, the finer the particle size, the larger the specific surface area and the higher the cost, and the smaller the mesh number of the filler can greatly save the cost.
According to the invention, various components in the formula are optimized in the sizing material, so that the sizing material has better construction application performance, the stripping performance between the coiled material and post-cast concrete is improved, the cost of the sizing material is not increased, economic support is provided for wide application of the sizing material in the market, and the wide application of the S-CLF YC waterproof coiled material is facilitated.
In addition, the invention also provides a preparation method of the sizing material for improving the stripping performance and the construction applicability of the S-CLF YC type coiled material, which comprises the following steps:
(5) mixing the oil product and the asphalt uniformly at the temperature of 100-130 ℃;
(6) heating the mixture obtained in the step (1) to 160-170 ℃, and then adding SBS under the stirring condition and mixing uniformly;
(7) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and uniformly mixing;
(8) grinding the mixed system obtained in the step (3) and continuously stirring to make the ground system more uniform;
(5) and (4) adding a filler into the mixed system ground in the step (4), uniformly stirring, cooling to room temperature, and finally discharging to obtain the rubber material.
According to the invention, the viscosity of the system in the preparation process is kept in a proper range by controlling the addition sequence of the raw materials which needs to be strictly controlled, so that the stirring process is easier to realize, a part of cost is saved, and the system is more uniform.
Preferably, in the above production method, the grinding is performed by a colloid mill and is carried out until the particle size of the material is 0.2 to 0.8 mm. The components with thicker particles are fully ground through a colloid mill, and the coarse particles are ground into fine particles while fully mixed, so that the modification effect is further improved.
Preferably, in the above preparation method, the asphalt is preheated before being added into the reaction system to keep the temperature between 100 ℃ and 130 ℃ so that the asphalt can be added into the system in a pumpable state, thereby shortening the preparation time.
The preparation process is based on the characteristics and combination of the raw materials in the formula, and through a large number of experiments and specific setting, the raw materials can be fully and uniformly mixed without agglomeration, so that the obtained sizing material has good performance.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to research, the butyl rubber, the lignin and the tackifying resin are matched with the oil product and the asphalt for use, so that the stripping performance of the rubber material and the post-cast concrete is improved, the construction is more convenient and faster, the appearance is more attractive, and the whole construction applicability is improved.
(2) According to the invention, the lignin, the tackifying resin and the butyl rubber are used in a matching manner, so that the adhesive force between the rubber material and mineral aggregate such as colored sand is obviously improved, the phenomenon that the mineral aggregate is easy to fall off is avoided, and the lignin in the rubber material is dispersed in the asphalt mixture in a three-dimensional manner, so that the function of reinforcing the asphalt mixture can be achieved; free oil in the rubber material can be fully absorbed, so that the produced rubber material has no oil separated out under high temperature conditions such as summer and the like, and the yellowing and blackening phenomena are prevented; meanwhile, after the lignin is added into the asphalt, the flow of the asphalt is prevented, the holding power to the asphalt is very strong, and the high-temperature resistance of the rubber material is also improved.
(3) Through a large amount of experimental researches, the inventor selects and compounds various raw materials, particularly properly uses butyl rubber, lignin and tackifying resin, and the rubber material has excellent stripping performance through the combination and compounding of the components, so that the stripping performance of an S-CLF coiled material and post-cast concrete is good, the problem that the stripping strength of an S-CLF YC waterproof coiled material and the post-cast concrete has defects is solved, and the parameter requirements in the enterprise standard Q/320584PAI011-2019 are met.
(4) The rubber material has low cost and simple preparation method, does not need to change the existing equipment, can be produced in large scale and is beneficial to wide application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments, but the scope of the present invention is not limited to the embodiments.
The starting materials used in the following examples are all commercially available unless otherwise specified.
Wherein the content of the first and second substances,
the asphalt is ordinary road asphalt, No. 90, available from petroleum and gas group, Inc. of China, and before use, the temperature of the asphalt is first raised to 115 ℃ to maintain the pumpable state of the asphalt.
The oil product is selected from heavy aromatic oil, specifically 60# oil product produced by Baozhenjin Daizhi Co., Ltd, and 35# oil product produced by Ahui Oriental belief building materials science and technology Co., Ltd.
SBS is thermoplastic styrene-butadiene rubber, is available from 3411 of Qiyang industry Limited of Huizhou city for SBS, and its number average molecular weight is 25 ten thousand daltons, and the weight of styrene block accounts for 30% of the total weight of SBS.
SBR is 92% SBR available from traded, Inc. of Gao's family, Shandong.
The lignin is obtained from WANTONG fiber technology limited of salt City
The tackifying resin is C5 series resin HHP-1204 produced by Beijing Hua Lin Rui Ci Co.
Wax powder is available from Changzhou Corsai successful Plastic Material Co., Ltd
The filler for the following examples was talc, which was a 200 mesh talc available from Tianyi calcium corporation, Huzhou.
Preparation of butyl rubber
Heating 42kg of 150# aromatic oil to 155 ℃, adding 35kg of 1502 styrene-butadiene rubber and 5kg of SBS, stirring for 30min at the rotating speed of 1000rpm, raising the temperature of a mixed system to 180 ℃ and stirring for 3h at the rotating speed of 1500rpm, adding 2kg of wax powder and stirring for 0.5h at the rotating speed of 1500rpm, grinding until no particles exist in the system, adding 16kg of 200-mesh talcum powder, stirring for 1h to uniformly mix the system, and cooling to room temperature to obtain the butyl rubber.
The butyl rubbers used in the following examples are all butyl rubbers prepared by the present preparation process.
Preparation examples
Preparation of example 1
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 100min at the temperature of 165 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.3mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A1.
Preparation of example 2
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 165 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 120min at the temperature of 165 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.3mm and continuing stirring for 10 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A2.
Preparation of example 3
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 170 ℃, and then adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 150min at the temperature of 165 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.5mm and continuing stirring for 10 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A3.
Preparation of example 4
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 110 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuing to add butyl rubber, SBR, lignin, tackifying resin and filler and stirring for 130min at the temperature of 165 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.4mm and continuing stirring for 20 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 70min to uniformly mix the system, cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A4.
Preparation of example 5
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 130min at the temperature of 160 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.6mm and continuing stirring for 20 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 80min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A5.
Preparation of example 6
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 175 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 100min at the temperature of 160 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.5mm and continuing stirring for 20 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 80min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A6.
Preparation of example 7
The composition of each raw material of the rubber compound is shown in the following table 1, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 115 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 150min at the temperature of 160 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.7mm and continuing stirring for 20 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 80min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain the rubber material, wherein the rubber material is marked as A7.
TABLE 1 amounts of the respective components in preparation examples 1 to 7
Figure BDA0003447731250000121
Comparative examples
Comparative example 1
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) adding SBR, lignin, tackifying resin and filler, and stirring for 100min at 165 ℃ to mix uniformly;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.4mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B1.
Comparative example 2
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 170 ℃, and then adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, tackifying resin and filler, and stirring for 120min at the temperature of 175 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.4mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B2.
Comparative example 3
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 165 ℃, adding SBS under stirring and mixing uniformly;
(3) continuing to add butyl rubber, SBR, lignin and filler and stirring for 100min at the temperature of 165 ℃ to uniformly mix the components;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.4mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 70min to uniformly mix the system, cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B3.
Comparative example 4
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuing to add SBR and filler and stirring for 100min at the temperature of 165 ℃ to uniformly mix the materials;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.5mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B4.
Comparative example 5
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 115 ℃;
(2) heating the mixture obtained in the step (1) to 165 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 150min at the temperature of 165 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.5mm and continuing stirring for 10 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 60min to uniformly mix the system, then cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B5.
Comparative example 6
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 150min at the temperature of 160 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.6mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 50min to uniformly mix the system, cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B6.
Comparative example 7
The specific raw material composition of the compound is shown in the following table 2, and the preparation method comprises the following steps.
(1) Mixing the oil product and the asphalt uniformly at 120 ℃;
(2) heating the mixture obtained in the step (1) to 160 ℃, adding SBS under stirring and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and stirring for 120min at the temperature of 175 ℃ to uniformly mix;
(4) grinding the mixed system obtained in the step (3) to a particle size of 0.6mm and continuing stirring for 5 min;
(5) and (3) adding talcum powder into the mixed system ground in the step (4), stirring for 40min to uniformly mix the system, cooling to room temperature, and finally discharging to obtain a rubber material, wherein the rubber material is marked as B7.
TABLE 2 amounts of the respective components in comparative examples 1 to 7
Figure BDA0003447731250000151
Performance testing
Test preparations 1 to 7 and comparative examples 1 to 7 the compounds prepared in the following examples were subjected to the following performance tests in accordance with the following criteria.
Preparation of a test piece: coating the S-CLF YC type coiled material on two surfaces of the S-CLF film by using sizing materials, wherein the thickness of the S-CLF YC type coiled material is controlled to be 0.5-0.8 mm; one surface of the waterproof roll is coated with a PE black film, the other surface of the waterproof roll is uniformly heated by a hot air gun after being cooled, and the waterproof roll is coated with colored sand, so that the S-CLF YC waterproof roll is prepared.
Viscosity: the viscosity test method uses a Brookfield viscometer method (rotational viscosity of asphalt) to measure, and the average of 3 readings is used as a measured value.
Softening point: the tests were carried out according to the standard methods specified in GBT 4507-2014.
Penetration degree: the tests were carried out according to the standard methods specified in GB/T4509-1998.
Oil permeability: removing an anti-sticking material PE black film on the lower surface of a test piece, placing the rubber surface downwards on 5 layers of medium-speed qualitative filter paper with the area larger than that of the test piece, then sealing and wrapping the filter paper and the test piece by using an aluminum foil, horizontally placing the test piece on a glazed brick pad, placing the filter paper below, pressing a 1kg weight on the test piece, placing the weight contact surface larger than the size of the test piece, then placing the test piece in an oven with the temperature adjusted to (80 +/-2) DEG C, horizontally placing for 24h +/-15 min, then placing the test piece at (23 +/-2) DEG C for 1h, and checking the number of oil seepage. The filter paper having the stain trace was measured as bleeding, and the number of bleedout was the largest among 3 specimens as a test result.
Low temperature: the test was carried out with reference to the low temperature flexibility test method specified in GB/T328.14-2007.
Heat resistance: a heat resistance test is carried out by referring to a method B in GB/T328.15-2007, and whether the test piece has slippage, flowing and falling is observed after the test is finished.
Peeling strength of coiled material post-cast concrete: test methods the tests were carried out according to the method specified in the trade designation Q/320584PAI011-2019, the specific test specimens being prepared as follows:
the production is carried out on an asphalt coiled material production line, a strong crossed membrane is arranged in the middle, the two sides are respectively the rubber materials prepared in the preparation examples 1-7 and the comparative examples 1-7, one side is well isolated by a silicone oil isolating membrane, the other side is isolated by standard sand, the thickness of the rubber material on one side of the silicone oil isolating membrane is 0.6mm, and the thickness of the rubber material on the side of a sand-coated layer is 0.5mm, so that the modified asphalt coiled material is prepared.
The untreated coiled material is prepared according to the sample preparation standard of the peel strength of the modified asphalt waterproof coiled material and the post-cast concrete, and the mixing ratio of cement mortar is 42.5 of strength grade ordinary portland cement: ISO standard sand: water 1: 2: 0.4, the size of the bonding surface of the test piece is (70 x 50) mm, a plurality of test pieces are prepared simultaneously by pouring mortar on a large block of coiled material, and the test piece is cut to the specified size before a peeling test. And (3) flatly placing the test piece at the bottom of the mould with the bonding surface facing upwards, pouring the cement mortar mixture into the mould, and compacting for 20s on a concrete vibration table according with JG/T245 specification, wherein the thickness is 30 mm-50 mm. And (5) placing at the temperature of (20 +/-2) ℃ for 24h, demolding, and curing under standard curing conditions for 168 h.
When the test piece is maintained, the test piece is placed in a room (23 +/-2) DEG C for 4h, a cement mortar board is arranged on a clamp at one end of a testing machine, one end of the coiled material which is not bonded is turned over by 180 degrees and is clamped in a clamp at the other end of the testing machine, the longitudinal axis of the test piece is coincided with the axes of the tensile testing machine and the clamp, the distance between the clamps is at least 100mm, and the pre-load is not born. The test was carried out at (23. + -.2) ° C, and the tensile rate was (100. + -.10) mm/min, and was continuously recorded until the test piece was separated.
The peeling strength of the heat-treated coiled material and the post-cast concrete needs to be realized by putting the prepared waterproof coiled material into an oven with the temperature of 80 ℃ for 7 days, taking out the coiled material and placing the coiled material at the temperature of 23 +/-2 ℃ for one day. Then, the sample was prepared, cured and tested as in the untreated case.
The peeling strength of the soaked coiled material and the post-cast concrete needs to be tested by preparing a sample of the untreated coiled material according to the sample preparation standard of the peeling strength of the modified asphalt waterproof coiled material and the post-cast concrete, maintaining the sample for 168 hours under the standard condition, putting the sample into water for 28 days, and then testing the performance.
Workability (appearance): cutting the prepared test piece into sample blocks of 300 multiplied by 300mm, respectively placing the sample blocks outdoors for 7 days and soaking the sample blocks in water for 7 days according to the test conditions of construction applicability, placing the sample blocks in an oven for 1 day, 7 days and 14 days at the temperature of 80 ℃, taking the sample blocks out, and observing the dropping condition of colored sand on the surface of the test piece, the oil spreading condition of a sand surface and an asphalt surface, and the sinking and blackening degree of the sand surface.
The test results are shown in tables 3, 4 and 5 below.
TABLE 3 basic Performance test results
Figure BDA0003447731250000171
TABLE 4 test results of peel strength of sizing material and post-cast concrete
Figure BDA0003447731250000172
Figure BDA0003447731250000181
TABLE 5 test results of sizing material application
Figure BDA0003447731250000182
Figure BDA0003447731250000191
As can be seen from the test data of the rubber compound prepared in comparative example 1, under the conditions that butyl rubber is not added or the addition amount of the butyl rubber is small and the addition amounts of lignin and tackifying resin are small, each item of stripping data of the coiled material is small and can not meet the standard requirement; meanwhile, the problem of applicability of the coiled material in construction is not solved, and the situations of yellowing and sand surface sinking are serious. From the performance test data of the rubber compounds prepared in comparative examples 2-4, it can be seen that under the condition that the single components of the lignin, the tackifying resin and the butyl rubber are not added or are not added at all, the change of the addition amounts of the SBS and the SBR has large influence on the viscosity of the coiled material, the high and low temperature and the peeling strength of the coiled material are not obviously improved, and the improvement degree on the construction applicability is low. From the performance test data of the rubber compound prepared in comparative example 5, it is seen that the performance and the construction applicability of the coil are not obviously improved under the conditions that the proportion of the lignin and the tackifying resin is small and the addition amount is small. As can be seen from the performance test data of the sizing material prepared in comparative example 6, the excessive addition of the lignin causes the excessive viscosity of the sizing material, which is not beneficial to the production, but the effect of the lignin on the stripping performance of the sizing material is obviously reflected, and all stripping strengths meet the standard requirements. From the performance test data of the sizing materials prepared in the preparation examples 1 to 7, the performance of the sizing material produced under the coordination of a proper amount of each component meets the actual use requirement, particularly, each stripping performance meets the standard requirement and has a certain margin, the construction applicability is also solved, and the defects that the surface color sand of the existing S-CLF YC waterproof coiled material is easy to fall off, the local part is yellow and black, and the appearance is poor can be overcome.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (10)

1. The sizing material for improving the stripping performance and construction applicability of the S-CLF YC type coiled material is characterized by comprising the following components in parts by weight:
Figure FDA0003447731240000011
2. the composition according to claim 1, wherein the bitumen is one or more of 90# bitumen, 100# bitumen, 110# bitumen, most preferably 90# bitumen, particularly preferably 90# bitumen, available from the group of petrochemical companies, the group of petroleum and gas in china, and/or the SK group in korea.
3. The compound according to claim 1, characterized in that the oil is a heavy aromatic oil having a viscosity of less than 5000mpa.s and an aniline point of less than 45 ℃.
4. A compound according to claim 1, characterised in that the weight ratio of bitumen to oil is (3-6): 1.
5. the rubber compound according to claim 4, wherein the butyl rubber is composed of 1502 styrene-butadiene rubber, aromatic oil, SBS, wax powder and talc, wherein the talc has a mesh number of 150-250 meshes.
6. The compound of claim 1, wherein the lignin is a modified lignin such as sulfonated lignin, phenolated lignin, or unmodified lignin.
7. The compound according to claim 1, wherein the tackifying resin is one or a mixture of two or more of coumarone resin, terpene resin, rosin resin, petroleum resin, phenol-formaldehyde resin epoxy resin and xylene-formaldehyde resin.
8. The rubber compound according to claim 1, wherein the filler is one or more of talc, fly ash, ground calcium carbonate, and light calcium carbonate.
9. Rubber compound according to claim 1, characterized in that the particle size of the filler is smaller than 250 mesh, more preferably between 150 and 200 mesh.
10. A process for the preparation of a compound according to any one of claims 1 to 9, characterized in that it comprises the following steps:
(1) mixing the oil product and the asphalt uniformly at the temperature of 100-130 ℃;
(2) heating the mixture obtained in the step (1) to 160-170 ℃, and then adding SBS under the stirring condition and mixing uniformly;
(3) continuously adding butyl rubber, SBR, lignin, tackifying resin and filler, and uniformly mixing;
(4) grinding the mixed system obtained in the step (3) and continuously stirring to make the ground system more uniform;
(5) and (4) adding a filler into the mixed system ground in the step (4), uniformly stirring, cooling to room temperature, and finally discharging to obtain the rubber material.
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