CN108068419A - A kind of lignin modified asphalt waterproof roll and preparation method thereof - Google Patents

A kind of lignin modified asphalt waterproof roll and preparation method thereof Download PDF

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Publication number
CN108068419A
CN108068419A CN201711167417.7A CN201711167417A CN108068419A CN 108068419 A CN108068419 A CN 108068419A CN 201711167417 A CN201711167417 A CN 201711167417A CN 108068419 A CN108068419 A CN 108068419A
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parts
modified
lignin
modified asphalt
waterproof roll
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CN201711167417.7A
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Inventor
刘拥军
刘永刚
郑新国
郑爱彬
候尚春
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Guangxi Wuxuan Jinpai Waterproof Material Science And Technology Co Ltd
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Guangxi Wuxuan Jinpai Waterproof Material Science And Technology Co Ltd
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Priority to CN201711167417.7A priority Critical patent/CN108068419A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • 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
    • B32B13/00—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material
    • B32B13/04—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material comprising such water setting substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B13/12—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material comprising such water setting substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • 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
    • B32B13/00—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material
    • B32B13/14—Layered products comprising a a layer of water-setting substance, e.g. concrete, plaster, asbestos cement, or like builders' material next to a fibrous or filamentary layer
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • 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
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • 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
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0276—Polyester fibres
    • 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
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/552—Fatigue strength
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/582—Tearability
    • B32B2307/5825—Tear resistant
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/73—Hydrophobic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Civil Engineering (AREA)
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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Road Paving Structures (AREA)

Abstract

A kind of lignin modified asphalt waterproof roll, the waterproof roll are five layered structures, are followed successively by from top to bottom：Upper surface separation layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modified asphalt layer and lower modified asphalt layer are made by modified pitch, and the modified pitch is to be prepared from the following raw materials in parts by weight：40 50 parts of phenolate lignin；20 25 parts of SBS modifier；50 60 parts of 90# asphalt；5 10 parts of silane coupling agent；58 parts of modified nano calcium carbonate；58 parts of tributyl phosphate；69 parts of polyvinyl alcohol；69 parts of aerosil；35 parts of sodium carboxymethylcellulose.The performances such as tearing toughness, caking property, water resistance, resistance to ag(e)ing and the high temperature resistant of the waterproof roll that present invention production obtains and saline-alkali tolerant are all greatly improved, and have higher elongation at break, and manufacture craft is simple.

Description

A kind of lignin modified asphalt waterproof roll and preparation method thereof
Technical field
The present invention relates to a kind of polymer membranes, more particularly, to a kind of lignin modified asphalt waterproof roll and its Production method belongs to waterproof chemistry Material Field.
Background technology
Asphalt has good caking property, ageing resistance and waterproof ability, be widely used as building the road for a long time, The materials such as waterproof and sealing.It is domestic and international waterproof, seepage control engineering the advantages of having raw material to be easy to get for waterproofing work, is cheap etc. In one of the material that is most widely used.
And economize on resources, environmental protection be China fundamental state policy.Lignin nature be only second to cellulose Two big natural organic-compounds.Global pulp and paper industry can generate about 50,000,000 tons of industrial lignins every year.China's system It is about 5,000,000,000 tons to starch paper waste discharge capacity, occupies the first place of China's all types of industries discharge capacity, pollution of the paper industry to water environment It is the most serious.According to statistics, county of China and county's more than papermaking and paper products industry wastewater discharge account for national industrial total release 18.6%, wherein processing emission compliance amount accounts for the 49.3% of paper-making industrial waste water total release.But current paper industry accounts for arranging The waste water for putting total amount 50% not yet carries out processing up to standard.And containing substantial amounts of lignin in paper waste, therefore annual papermaking is produced Raw lignin is also up to 4,500,000 tons.Due to the limitation of its own some intrinsic characteristic and current economic technology condition, so far Until, only only 6% or so industrial lignin is utilized effectively, after the concentration of most lignin as fuel burn-up or It is directly discharged into rivers.This not only causes the significant wastage of resource, but also has seriously polluted the environment.To solve energy shortage, people Stepping up to develop biomass alcohol fuel.In the production process of biomass ferment ethyl alcohol, lignin and cellulose and Hemicellulose is different, after experience dilute acid pretreatment, saccharification and fermentation step, it is impossible to and fermentable sugars is converted into, is solid residue, Necessarily lead to substantial amounts of lignin byproduct in wood-based composites biofuel production process, biology will be directly affected by efficiently using The economic competitiveness of matter ethyl alcohol.
It is as follows that applicant retrieves the pertinent literature being modified to pitch as modifying agent by the use of lignin：
Application number：201310647897.2；Applicant：Hohai University；Denomination of invention：Lignin modified asphalt and preparation method thereof And application；Summary：Lignin modified asphalt and its preparation method and application, the present invention are prepared by following steps：(1) it is wooden The extraction of element；(2) lignin is refined；(3) modification of lignin；(4) by modified lignin resin obtained by step (3) and asphalt It is placed in reaction vessel, adds in Na2S reacts 30min, post-treated to obtain lignin modified asphalt.The present invention is black from discarded papermaking Lignin is extracted in liquid, and chemical modification is carried out to pitch using refined modified lignin, obtains lignin modified asphalt, The corrosion resistance of modified pitch is suitable with pitch before modified, and elastic restoration ratio is high by 1.2% compared with pitch before modified, Viscosity at identical temperature is higher than the viscosity of unmodified preceding pitch, therefore the performance phase of lignin modified asphalt and unmodified pitch When, therefore pitch can be replaced with lignin modified asphalt, petroleum resources are not only effectively saved, but also two have been carried out to discarded black liquid Secondary utilization.
Application number：200810011462.8；Applicant：Sinopec Group；Sinopec's stock Fushun Petrochemical Research Institute of part Co., Ltd；Denomination of invention：A kind of lignin modified asphalt composition and preparation method thereof；It plucks It will：The invention discloses a kind of lignin modified asphalt compositions and preparation method thereof.The bituminous composition is by 60% ~ 98% Residual oil and/or pitch, 1% ~ 30% lignin, 0.5% ~ 10.0% stabilizer composition, wherein stabilizer is tapped oil and/or coal tar Oil.The present invention is stabilizer using tapped oil and/or coal tar, can make lignin uniformly, be dispersed stably in pitch, can be with Sinking speed of the lignin in pitch is substantially reduced, the stability of lignin modified asphalt is improved, is conducive to lignin modification The industrialized production of pitch.
Two patents mentioned above, although all having carried out being modified to obtain performance more preferably lignin modification drip to pitch Blue or green composition, but its effect is in order to which lignin is made to be stable in the presence of in pitch, lignin and pitch do not carry out chemistry Reaction, modified asphalt composite adhesion strength be not strong.Therefore, for this defect, the present inventor is based on being engaged in such waterproof volume Material design abundant for many years practical experience and professional knowledge, and coordinate the utilization of scientific principle, actively it is subject to research and innovation, to found A kind of lignin modified asphalt waterproof roll and its production method can improve general existing lignin modified asphalt combination Object makes it with more practicability and enhances its adhesion strength.By constantly studying, designing, and through studying sample repeatedly and changing Into rear, created finally with the high present invention of practical value and adhesion strength.
The content of the invention
For above-mentioned technological deficiency, the purpose of the present invention is develop a kind of lignin modified asphalt waterproof roll and Its production method using the group at silane coupling agent both ends, forms " molecular link bridge " between lignin and pitch matrix, passes through Chemical bonding acts on, and enhances the interface binding power of lignin and pitch, and makes modified pitch coupling into reactivity Macromolecular, this macromolecular plays chemical crosslink reaction with concrete jointly and physics mortise and tenon cooperates with cementation.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of lignin modified asphalt waterproof roll, the waterproof roll are five layered structures, are followed successively by from top to bottom：Upper surface every Absciss layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modified asphalt layer changes under Property bitumen layer is made by modified pitch, and the modified pitch is to be prepared from the following raw materials in parts by weight：Phenolate lignin 40-50 parts；20-25 parts of SBS modifier；50-60 parts of 90# asphalt；5-10 parts of silane coupling agent；Modified nano calcium carbonate 5- 8 parts；5-8 parts of tributyl phosphate；6-9 parts of polyvinyl alcohol；6-9 parts of aerosil；3-5 parts of sodium carboxymethylcellulose.
The upper surface separation layer is one kind in polyethylene film, precoated sand or polyesters isolation film, and lower surface isolates Layer is polyethylene film；The tire base is one in polyester fiber non-woven fabric, HDPE film, glass fiber felt or fiberglass reinforcing polyester felt Kind.
The preparation method of the modified nano calcium carbonate is：Nano-calcium carbonate calcium powder is dry in 115~120 DEG C of dehydrations It is dry, it is then added in high-speed mixer, stirs and heat up, 90 DEG C stop heating, add in the chelating of nano-calcium carbonate quality 2.0% Type titanate coupling agent KR-201, in 90 DEG C of modified 10min；Add in one by one again nano-calcium carbonate quality 2.0% stearic acid, 0.5% coconut oil and 1% technical white oil are modified 10~15 min respectively again at 90 DEG C, shut down, discharging, obtain modification and receive Rice calcium carbonate.
The silane coupling agent for diethylenetriamine base propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, γ-ethylenediamine ethyl triethoxy silicane alkane, three tert-butoxy vinyl silanes, N- methyl -3- aminopropyl trimethoxysilanes, γ - Methyl allyl acyloxypropyl trimethoxysilane, γ-ureidopropyltriethoxysilane, (3- aminopropyls) triethoxysilicane One or more in alkane, N- phenyl -3- TSL 8330s.
Lignin modified asphalt waterproof roll, production method include the following steps：
1）First prepare phenolate lignin：
Sodium lignin sulfonate is added in heating reaction kettle, adds in the phenol solution of sodium lignin sulfonate weight 60%, stirring is equal Even, the mass concentration for adding sodium lignin sulfonate weight 3-5% is the sodium hydroxide solution of 40-50%, and stirring and dissolving is warming up to 110-120 DEG C, constant temperature be stirred to react 0.8-2 it is small when after, with hydrochloric acid adjust reaction solution pH=2-3, filter, wash filter cake with boiling water Until no free-phenol exists, phenolate lignin is obtained；Phenolate lignin is ground into granularity less than or equal to 1 li with mill Rice；
2）Prepare modified pitch：
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 140-160 DEG C, Add in step 1）The phenolate lignin and silane coupling agent of parts by weight, after being stirred 60-90 minutes with high-speed shearing machine, then will The temperature of reaction kettle is warming up to 175-180 DEG C, adds in the SBS modifier of parts by weight in a kettle, and stirring is melted uniformly, Obtain mixture A；Then in parts by weight by modified nano calcium carbonate, polyvinyl alcohol, aerosil and carboxymethyl cellulose Sodium is added sequentially in mixture A, using high-speed shearing machine that the material stirring of addition is uniform, mixture B；Again to mixture B The middle tributyl phosphate for adding in parts by weight, mixes uniformly, all materials in reaction kettle is carried out again on high-speed shearing machine Until 90# asphalt is uniformly dispersed with unclassified stores, modified pitch is made in shearing 90~110 minutes；
3）Through forming technology of coiled material, tire base is placed in centre, by step（2）Modified pitch obtained is uniformly coated on tire base Upper and lower surface, be then covered with upper surface separation layer and lower surface separation layer, then cooled down through cooling device, count length, trimming, receipts It rolls up, pack to obtain finished product.
The reaction principle of bitumen layer of the present invention is：Silane coupling agent is a kind of organic matter contained there are many functional group, The hydrolyzable alkoxy grp in one end is connected with the phenolic hydroxyl group of phenolate lignin, the organic functionals such as vinyl, amido of the other end Group and the carboxyl of pitch connect, and form " molecular link bridge " between phenolate lignin and pitch matrix, pass through chemical bonding Effect, enhances the interface binding power of lignin and pitch, and makes pitch coupling into the macromolecular with reactivity, this big When molecule is contacted with basal plane, modified pitch molecule section and concrete form physical absorption, and the macromolecular with reactivity with Chemical bonding suction-operated occurs for concrete, generates chemical interactions, therefore the waterproof layer and the cohesive force of concrete that are formed are just It greatly enhances, it is difficult to by extraneous such environmental effects.The present invention is layered in order to which product stabilization is made to be not easy isolation, it is also necessary to add Modified nano calcium carbonate, aerosil and antifoaming agent etc..Research shows the sodium lignin sulfonate active group after phenolate More, organic active is high, so allows between phenolate lignin and pitch there are chemical bonds, and untreated lignin It is mechanical interlocked that dependence is cohered between pitch, is only physics mortise and tenon.Therefore, phenolate treated sodium lignin sulfonate and pitch Interface bond strength is improved.
In the present invention, add in through chelating titanate coupling agent, stearic acid, coconut oil and technical white oil is modified receives Rice calcium carbonate, eliminates the cohesion of nano-calcium carbonate itself, and grain size becomes smaller, and distribution is more equal, contributes to nano-calcium carbonate poly- in height Homodisperse in object, modified nano-calcium carbonate and modified pitch bulk junction is strong with joint efforts, further improves the power of product Learn performance.Also, by inventor the study found that modified nano-calcium carbonate hydrophobic oleophilic oil, therefore by modified nano-meter caco 3 Calcium, which is added in the modified asphalt layer of the present invention, has preferable compatibility and dispersiveness.
The polyvinyl alcohol is a kind of stabilizer, can increase the stability of solution, colloid, solid, mixture.
The tributyl phosphate is a kind of paint solvent and antifoaming agent.It is difficult due to the low surface tension of tributyl phosphate The physical property of water is dissolved in, the film of established foam can effectively be made to be in an unsure state and defoam rapidly.
Sodium carboxymethylcellulose abbreviation CMC-Na used in the present invention is the cellulose that glucose polymerization degree is 100-2000 Derivative can play the role of anti-settling agent and dispersant in the present invention, and coating is made to have thixotropy, greatly improves viscosity, and It can prevent the sedimentation and cohesion of particle, be uniformly distributed, make coating not stratified for a long time.
Aerosil（It is commonly called as fume colloidal silica）It is through a kind of made from oxyhydrogen flame pyrohydrolysis using chlorosilane Finely, special amorphous powder body material, product purity are high, and Average primary grain size is about 7 ~ 40nm, and specific surface area 50 ~ 380m2/ g, SiO2Content >=99.8%.It is a kind of multi-functional additive, is widely used in coating, can play thickening, touch The effects that change, delustring.In the present invention, aerosil is used as thixotropic agent, because usually in the construction process, due to The solvent volatilization of coating edge is very fast, causes surface tension uneven, liquid is easily made to be moved to edge, and network of silica The movement of liquid can effectively be prevented and form webbing, while also prevent the sagging phenomenon of liquid in the curing process, make painting Layer is uniformly.Meanwhile aerosil be due to that can form hydrogen bond and the middle low-shear viscosity in raising system, so as to play thickening Act on therefore, aerosil being widely used in oleaginous system is general.After using thixotropic agent in coating, in construction High-rate of shear under have compared with low-viscosity, coating is contributed to flow and is easy to construct；Low sheraing speed before construction and afterwards Have under rate compared with high viscosity, can prevent pigment sedimentation and wet film sagging.In coating system, due to the small particle of aerosil And high surface energy, they can be adsorbed on the surface of fine paint powders, and form a surface layer in powder surface, improve point of powder Property is dissipated, therefore can be used as dispersion aids.In same coating system, when adding in aerosil can be obviously shortened scattered Between, improve production efficiency.Aerosil can also improve the weatherability of coating, resistance to marring, improve coating and base material it Between bond strength.Meanwhile aerosil has extremely strong ultraviolet radiation absorption, infrared light reflection characteristic, doses in coating The middle anti-aging property that can improve coating.
Compared with prior art, the positive effect of the present invention is：
1st, the upper modified asphalt layer of lignin modified asphalt waterproof roll of the present invention and lower modified asphalt layer are by lignin and idol The connection common modified pitch of agent is made, and when preparing lignin and coupling agent modified synergic pitch, utilizes the organic of silane coupling agent Active group, the hydrolyzable alkoxy grp of its one end are connected with the phenolic hydroxyl group of phenolate lignin, vinyl, the amido of the other end The carboxyl of organo-functional groups and pitch is waited to connect, " molecular link bridge " is formed between phenolate lignin and pitch matrix, is led to Chemical bonding effect is crossed, enhances the interface binding power of lignin and pitch, and makes pitch coupling into the big of reactivity Molecule, when this macromolecular is contacted with basal plane, modified pitch molecule section forms physical absorption with concrete, and with reactivity Macromolecular and concrete chemical bonding suction-operated occurs, generate chemical interactions, therefore the waterproof layer and concrete formed Cohesive force just greatly enhance, it is difficult to by extraneous such environmental effects.The present invention is layered in order to which product stabilization is made to be not easy isolation, Also need to addition modified nano calcium carbonate, aerosil, polyvinyl alcohol and sodium carboxymethylcellulose etc..
2nd, the lignin modified asphalt waterproof roll that the present invention is prepared is for strong with the bonding of building basal plane in building Degree is big, good water-proof effect.Lignin modified asphalt waterproof roll obtained is used to prepare the upper modification of waterproof roll by the present invention Bitumen layer and lower modified asphalt layer, this two layers of modified asphalt layer can play chemical crosslink reaction and physics mortise and tenon jointly with concrete Cementation is cooperateed with, can wriggle and be penetrated into cement gel and concrete pore during cement, concrete setting, be reached To be tightly combined, secured, irreversible as closely linked as flesh and blood bond effect, substantially increase the adhesion strength of waterproof roll.On and Modified asphalt layer and lower modified asphalt layer and the bonding of concrete surface are irreversible, adhesion strength is big, tearing toughness is high, Elongation percentage is big, even if basal plane expands with heat and contract with cold and generates that displacement is even cracked or adhesive surface is for a long time subject to immersion and the hydraulic pressure of water Effect, still keeps bond effect.
3rd, after the present invention is modified pitch by using SBS modifier, coupling agent and sodium lignin sulfonate, obtain Properties of Modified Asphalt is stablized, and adhesion strength is big；And aerosil is added, improves the weatherability of asphalt system and anti-ageing Change performance, add modified nano calcium carbonate, effectively improve the storage stability and dispersion performance of modified pitch system；It adds in Tributyl phosphate, makes the coating defoam rapidly；Polyvinyl alcohol is added in, keeps the stabilization of system；Add sodium carboxymethylcellulose, Make coating that there is thixotropy, greatly improve viscosity, and can prevent the sedimentation and cohesion of particle, be uniformly distributed.And the modification is dripped Green grass or young crops is used for that waterproof roll is made, and makes the tearing toughness of the waterproof roll of generation, caking property, water resistance, resistance to ag(e)ing and resistance to The performances such as high temperature are all greatly improved.
Specific embodiment
Embodiment 1
A kind of lignin modified asphalt waterproof roll, the waterproof roll are five layered structures, are followed successively by from top to bottom：Upper surface every Absciss layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modified asphalt layer changes under Property bitumen layer is made by modified pitch, and the modified pitch is to be prepared from the following raw materials in parts by weight：Phenolate lignin 40 parts；20 parts of SBS modifier；50 parts of 90# asphalt；5 parts of diethylenetriamine base propyl trimethoxy silicane；Modified Nano carbon Sour 5 parts of calcium；5 parts of tributyl phosphate；6 parts of polyvinyl alcohol；6 parts of aerosil；3 parts of sodium carboxymethylcellulose.
The upper surface separation layer is polyethylene film, and lower surface separation layer is polyethylene film；The tire base is poly- Ester fiber non-woven fabrics.
The preparation method of the modified nano calcium carbonate is：Nano-calcium carbonate calcium powder is dry in 115~120 DEG C of dehydrations It is dry, it is then added in high-speed mixer, stirs and heat up, 90 DEG C stop heating, add in the chelating of nano-calcium carbonate quality 2.0% Type titanate coupling agent KR-201, in 90 DEG C of modified 10min；Add in one by one again nano-calcium carbonate quality 2.0% stearic acid, 0.5% coconut oil and 1% technical white oil are modified 10~15 min respectively again at 90 DEG C, shut down, discharging, obtain modification and receive Rice calcium carbonate.
Lignin modified asphalt waterproof roll, production method include the following steps：
1）First prepare phenolate lignin：
Sodium lignin sulfonate is added in heating reaction kettle, adds in the phenol solution of sodium lignin sulfonate weight 60%, stirring is equal Even, the mass concentration for adding sodium lignin sulfonate weight 3% is 40% sodium hydroxide solution, and stirring and dissolving is warming up to 110 DEG C, constant temperature be stirred to react 2 it is small when after, with hydrochloric acid adjust reaction solution pH=2-3, filter, with boiling water wash filter cake until without dissociate benzene Phenol exists, and obtains phenolate lignin；Phenolate lignin is ground into granularity less than or equal to 1 centimetre with mill；
2）Prepare modified pitch：
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 140 DEG C, is added in Step 1）The phenolate lignin and silane coupling agent of parts by weight, after being stirred 60-90 minutes with high-speed shearing machine, then will reaction The temperature of kettle is warming up to 175 DEG C, adds in the SBS modifier of parts by weight in a kettle, and stirring melts uniformly, obtains mixture A；Then modified nano calcium carbonate, polyvinyl alcohol, aerosil and sodium carboxymethylcellulose are added successively in parts by weight Enter into mixture A, using high-speed shearing machine that the material stirring of addition is uniform, mixture B；Weight is added in into mixture B again Measure the tributyl phosphate of number, mix uniformly, all materials in reaction kettle are carried out on high-speed shearing machine again shearing 90~ 110 minutes, until 90# asphalt is uniformly dispersed with unclassified stores, modified pitch is made；
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 140 DEG C, is added in Step 1）The phenolate lignin of parts by weight and the diethylenetriamine base propyl trimethoxy silicane of above-mentioned parts by weight, with height Fast cutter stirs 60-90 minutes, obtains mixture A；In parts by weight by modified nano calcium carbonate, polyvinyl alcohol, gas phase dioxy SiClx and sodium carboxymethylcellulose are added sequentially in mixture A, using high-speed shearing machine that the material stirring of addition is uniform, are mixed Close object B；The tributyl phosphate of parts by weight is added in into mixture B again, is mixed uniformly, by all materials in reaction kettle at a high speed Shearing 90~110 minutes is carried out on cutter again, until 90# asphalt is uniformly dispersed with unclassified stores, modified drip is made It is blue or green；
3）Through forming technology of coiled material, tire base is placed in centre, by step（2）Modified pitch obtained is uniformly coated on tire base Upper and lower surface, be then covered with upper surface separation layer and lower surface separation layer, then cooled down through cooling device, count length, trimming, receipts It rolls up, pack to obtain finished product.
Embodiment 2
A kind of lignin modified asphalt waterproof roll, the waterproof roll are five layered structures, are followed successively by from top to bottom：Upper surface every Absciss layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modified asphalt layer changes under Property bitumen layer is made by modified pitch, and the modified pitch is to be prepared from the following raw materials in parts by weight：Phenolate lignin 45 parts；23 parts of SBS modifier；55 parts of 90# asphalt；2 parts of gamma-aminopropyl-triethoxy-silane；γ-three ethoxy of ethylenediamine base 3 parts of base silane；Three 3 parts of tert-butoxy vinyl silanes；7 parts of modified nano calcium carbonate；7 parts of tributyl phosphate；Polyvinyl alcohol 8 Part；8 parts of aerosil；34 parts of sodium carboxymethylcellulose.
The upper surface separation layer is precoated sand, and lower surface separation layer is polyethylene film；The tire base is HDPE Film.
The preparation method of the modified nano calcium carbonate is：Nano-calcium carbonate calcium powder is dry in 115~120 DEG C of dehydrations It is dry, it is then added in high-speed mixer, stirs and heat up, 90 DEG C stop heating, add in the chelating of nano-calcium carbonate quality 2.0% Type titanate coupling agent KR-201, in 90 DEG C of modified 10min；Add in one by one again nano-calcium carbonate quality 2.0% stearic acid, 0.5% coconut oil and 1% technical white oil are modified 10~15 min respectively again at 90 DEG C, shut down, discharging, obtain modification and receive Rice calcium carbonate.
Lignin modified asphalt waterproof roll, production method include the following steps：
1）First prepare phenolate lignin：
Sodium lignin sulfonate is added in heating reaction kettle, adds in the phenol solution of sodium lignin sulfonate weight 60%, stirring is equal Even, the mass concentration for adding sodium lignin sulfonate weight 4% is 45% sodium hydroxide solution, and stirring and dissolving is warming up to 115 DEG C, constant temperature be stirred to react 1.5 it is small when after, with hydrochloric acid adjust reaction solution pH=2-3, filter, with boiling water wash filter cake until without dissociate Phenol exists, and obtains phenolate lignin；Phenolate lignin is ground into granularity less than or equal to 1 centimetre with mill；
2）Prepare modified pitch：
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 150 DEG C, is added in Step 1）The phenolate lignin of parts by weight and the gamma-aminopropyl-triethoxy-silane of above-mentioned parts by weight, γ-ethylenediamine base 3 parts of triethoxysilane and three tert-butoxy vinyl silanes, after being stirred 60-90 minutes with high-speed shearing machine, then by reaction kettle Temperature be warming up to 178 DEG C, add in the SBS modifier of parts by weight in a kettle, stirring is melted uniform, obtains mixture A； Then modified nano calcium carbonate, polyvinyl alcohol, aerosil and sodium carboxymethylcellulose are sequentially added in parts by weight It is using high-speed shearing machine that the material stirring of addition is uniform into mixture A, mixture B；Again weight is added in into mixture B The tributyl phosphate of number is mixed uniformly, all materials in reaction kettle is carried out shearing 90~110 again on high-speed shearing machine Minute, until 90# asphalt is uniformly dispersed with unclassified stores, modified pitch is made；
3）Through forming technology of coiled material, tire base is placed in centre, by step（2）Modified pitch obtained is uniformly coated on tire base Upper and lower surface, be then covered with upper surface separation layer and lower surface separation layer, then cooled down through cooling device, count length, trimming, receipts It rolls up, pack to obtain finished product.
Embodiment 3
A kind of lignin modified asphalt waterproof roll, the waterproof roll are five layered structures, are followed successively by from top to bottom：Upper surface every Absciss layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modified asphalt layer changes under Property bitumen layer is made by modified pitch, and the modified pitch is to be prepared from the following raw materials in parts by weight：Phenolate lignin 50 parts；25 parts of SBS modifier；60 parts of 90# asphalt；2 parts of gamma-methyl allyl acyloxypropyl trimethoxysilane；γ-urea groups 1 part of propyl-triethoxysilicane；3 parts of (3- aminopropyls) triethoxysilane；N- phenyl -3- TSL 8330s 4 parts；8 parts of modified nano calcium carbonate；8 parts of tributyl phosphate；9 parts of polyvinyl alcohol；9 parts of aerosil；Carboxymethyl cellulose 5 parts of sodium.
The upper surface separation layer is polyesters isolation film, and lower surface separation layer is polyethylene film；The tire base For fiberglass reinforcing polyester felt.
The preparation method of the modified nano calcium carbonate is：Nano-calcium carbonate calcium powder is dry in 115~120 DEG C of dehydrations It is dry, it is then added in high-speed mixer, stirs and heat up, 90 DEG C stop heating, add in the chelating of nano-calcium carbonate quality 2.0% Type titanate coupling agent KR-201, in 90 DEG C of modified 10min；Add in one by one again nano-calcium carbonate quality 2.0% stearic acid, 0.5% coconut oil and 1% technical white oil are modified 10~15 min respectively again at 90 DEG C, shut down, discharging, obtain modification and receive Rice calcium carbonate.
Lignin modified asphalt waterproof roll, production method include the following steps：
1）First prepare phenolate lignin：
Sodium lignin sulfonate is added in heating reaction kettle, adds in the phenol solution of sodium lignin sulfonate weight 60%, stirring is equal Even, the mass concentration for adding sodium lignin sulfonate weight 5% is 50% sodium hydroxide solution, and stirring and dissolving is warming up to 120 DEG C, constant temperature be stirred to react 0.8 it is small when after, with hydrochloric acid adjust reaction solution pH=2-3, filter, with boiling water wash filter cake until without dissociate Phenol exists, and obtains phenolate lignin；Phenolate lignin is ground into granularity less than or equal to 1 centimetre with mill；
2）Prepare modified pitch：
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 160 DEG C, is added in Step 1）The phenolate lignin of parts by weight and the gamma-methyl allyl acyloxypropyl trimethoxysilane of above-mentioned parts by weight, γ-ureidopropyltriethoxysilane, (3- aminopropyls) triethoxysilane and N- phenyl -3- aminopropyl trimethoxy silicon Alkane is warming up to 180 DEG C after high-speed shearing machine stirring 60-90 minutes, then by the temperature of reaction kettle, adds in weight in a kettle The SBS modifier of number, stirring melt uniformly, obtain mixture A；Then in parts by weight by modified nano calcium carbonate, polyethylene Alcohol, aerosil and sodium carboxymethylcellulose are added sequentially in mixture A, using high-speed shearing machine by the material of addition It stirs evenly, mixture B；The tributyl phosphate of parts by weight is added in into mixture B again, is mixed uniformly, by the institute in reaction kettle There is material to carry out shearing 90~110 minutes again on high-speed shearing machine, until 90# asphalt disperses with unclassified stores It is even, modified pitch is made；
3）Through forming technology of coiled material, tire base is placed in centre, by step（2）Modified pitch obtained is uniformly coated on tire base Upper and lower surface, be then covered with upper surface separation layer and lower surface separation layer, then cooled down through cooling device, count length, trimming, receipts It rolls up, pack to obtain finished product.
Modified nano calcium carbonate produced by the invention and unmodified nano-calcium carbonate performance are compared, are modified Nano-calcium carbonate reduces 48.6% than unmodified nano-calcium carbonate oil factor, and settling volume reduces 57.6%, and viscosity reduces 59.9%, bulk density reduces 16.4%, illustrates modified nano-calcium carbonate oleophilic drainage, with lignin modified asphalt phase Capacitive is good, and bulk density becomes smaller, and illustrates that modified nano-calcium carbonate dispersion performance is good, is not easy to reunite.
The present invention and modified asphalt product experimental data comparison such as following table：
The lignin modified asphalt waterproof roll that the present invention is prepared is for big, anti-with the adhesion strength of building basal plane in building Water effect is good.The present invention by lignin modified asphalt waterproof roll obtained be used to prepare waterproof roll upper modified asphalt layer and Lower modified asphalt layer, this two layers of modified asphalt layer can play chemical crosslink reaction jointly with concrete and physics mortise and tenon cooperates with bonding Effect, can wriggle during cement, concrete setting and penetrate into cement gel and concrete pore, reach with reference to tight Close, secured, irreversible as closely linked as flesh and blood bond effect substantially increases the adhesion strength of waterproof roll.And upper modified pitch Layer and lower modified asphalt layer and the bonding of concrete surface are irreversible, and adhesion strength is big, tearing toughness is high, elongation percentage Greatly, even if basal plane expands with heat and contract with cold, generation displacement is even cracked or adhesive surface is subject to the immersion of water and acting on for hydraulic pressure for a long time, Still keep bond effect.

Claims (5)

1. a kind of lignin modified asphalt waterproof roll, it is characterised in that：The waterproof roll be five layered structures, from top to bottom according to It is secondary to be：Upper surface separation layer, upper modified asphalt layer, tire base, lower modified asphalt layer and lower surface separation layer；The upper modification Bitumen layer and lower modified asphalt layer are made by modified pitch, and the modified pitch is by the raw material system of following parts by weight Into：40-50 parts of phenolate lignin；20-25 parts of SBS modifier；50-60 parts of 90# asphalt；5-10 parts of silane coupling agent；Change 5-8 parts of nano-calcium carbonate of property；5-8 parts of tributyl phosphate；6-9 parts of polyvinyl alcohol；6-9 parts of aerosil；Carboxymethyl cellulose Plain sodium 3-5 parts.
2. lignin modified asphalt waterproof roll according to claim 1, it is characterised in that：The upper surface separation layer For one kind in polyethylene film, precoated sand or polyesters isolation film, lower surface separation layer is polyethylene film；The tire base is One kind in polyester fiber non-woven fabric, HDPE film, glass fiber felt or fiberglass reinforcing polyester felt.
3. lignin modified asphalt waterproof roll according to claim 1, it is characterised in that：The modified nano-meter caco 3 The preparation method of calcium is：By nano-calcium carbonate calcium powder in 115~120 DEG C of dehydration and drying, it is then added in high-speed mixer, stirs It mixes and heats up, 90 DEG C stop heating, the chelating titanate coupling agent KR-201 of nano-calcium carbonate quality 2.0% are added in, 90 DEG C modified 10min；Add in stearic acid, 0.5% coconut oil and 1% technical white oil of nano-calcium carbonate quality 2.0% one by one again, It is modified 10~15 min respectively again at 90 DEG C, shuts down, discharging obtains modified nano calcium carbonate.
4. lignin modified asphalt waterproof roll according to claim 1, it is characterised in that：The silane coupling agent is Diethylenetriamine base propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, γ-ethylenediamine ethyl triethoxy silicane alkane, three Tert-butoxy vinyl silanes, N- methyl -3- aminopropyl trimethoxysilanes, gamma-methyl allyl acyloxypropyl trimethoxy silicon Alkane, γ-ureidopropyltriethoxysilane, (3- aminopropyls) triethoxysilane, N- phenyl -3- aminopropyl trimethoxies One or more in silane.
5. lignin modified asphalt waterproof roll, it is characterised in that：Its production method includes the following steps：
1）First prepare phenolate lignin：
Sodium lignin sulfonate is added in heating reaction kettle, adds in the phenol solution of sodium lignin sulfonate weight 60%, stirring is equal Even, the mass concentration for adding sodium lignin sulfonate weight 3-5% is the sodium hydroxide solution of 40-50%, and stirring and dissolving is warming up to 110-120 DEG C, constant temperature be stirred to react 0.8-2 it is small when after, with hydrochloric acid adjust reaction solution pH=2-3, filter, wash filter cake with boiling water Until no free-phenol exists, phenolate lignin is obtained；Phenolate lignin is ground into granularity less than or equal to 1 li with mill Rice；
2）Prepare modified pitch：
90# asphalt is added in reaction heating kettle according to parts by weight, after reaction temperature is heated to 140-160 DEG C, Add in step 1）The phenolate lignin and silane coupling agent of parts by weight, after being stirred 60-90 minutes with high-speed shearing machine, then will The temperature of reaction kettle is warming up to 175-180 DEG C, adds in the SBS modifier of parts by weight in a kettle, and stirring is melted uniformly, Obtain mixture A；Then in parts by weight by modified nano calcium carbonate, polyvinyl alcohol, aerosil and carboxymethyl cellulose Sodium is added sequentially in mixture A, using high-speed shearing machine that the material stirring of addition is uniform, mixture B；Again to mixture B The middle tributyl phosphate for adding in parts by weight, mixes uniformly, all materials in reaction kettle is carried out again on high-speed shearing machine Until 90# asphalt is uniformly dispersed with unclassified stores, modified pitch is made in shearing 90~110 minutes；
3）Through forming technology of coiled material, tire base is placed in centre, by step（2）Modified pitch obtained is uniformly coated on tire base Upper and lower surface, be then covered with upper surface separation layer and lower surface separation layer, then cooled down through cooling device, count length, trimming, receipts It rolls up, pack to obtain finished product.
CN201711167417.7A 2017-11-21 2017-11-21 A kind of lignin modified asphalt waterproof roll and preparation method thereof Withdrawn CN108068419A (en)

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CN112895527A (en) * 2021-03-02 2021-06-04 潍坊市宇虹防水材料(集团)有限公司 Preparation method of high-temperature-resistant modified asphalt waterproof coiled material and waterproof coiled material

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CN107175870A (en) * 2016-03-09 2017-09-19 广西金雨伞防水装饰有限公司 Strengthen the modified asphalt waterproof coiled material and its production method of overlap edge
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