CN105733490A - Moisture-curable self-cross-linked cement concrete pavement joint sealant - Google Patents
Moisture-curable self-cross-linked cement concrete pavement joint sealant Download PDFInfo
- Publication number
- CN105733490A CN105733490A CN201610175923.XA CN201610175923A CN105733490A CN 105733490 A CN105733490 A CN 105733490A CN 201610175923 A CN201610175923 A CN 201610175923A CN 105733490 A CN105733490 A CN 105733490A
- Authority
- CN
- China
- Prior art keywords
- concrete pavement
- cross
- hydroxyl
- cemcent
- joint sealant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004568 cement Substances 0.000 title claims abstract description 22
- 239000000565 sealant Substances 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 32
- 238000004132 cross linking Methods 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 11
- 239000012948 isocyanate Substances 0.000 claims abstract description 9
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 9
- 239000000049 pigment Substances 0.000 claims abstract description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 8
- 229920000570 polyether Polymers 0.000 claims abstract description 8
- 229920005862 polyol Polymers 0.000 claims abstract description 8
- 150000003077 polyols Chemical class 0.000 claims abstract description 8
- 229920000587 hyperbranched polymer Polymers 0.000 claims abstract 3
- 238000006243 chemical reaction Methods 0.000 claims description 75
- 229920000642 polymer Polymers 0.000 claims description 34
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 28
- -1 methyl siloxane Chemical class 0.000 claims description 25
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 21
- 239000000945 filler Substances 0.000 claims description 17
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 239000004014 plasticizer Substances 0.000 claims description 8
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 8
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 8
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 238000001723 curing Methods 0.000 claims description 6
- 238000013008 moisture curing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 14
- 229920002635 polyurethane Polymers 0.000 abstract description 11
- 239000004814 polyurethane Substances 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 8
- 239000010703 silicon Substances 0.000 abstract description 8
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 abstract description 4
- 241001112258 Moca Species 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 230000000711 cancerogenic effect Effects 0.000 abstract 1
- 231100000315 carcinogenic Toxicity 0.000 abstract 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 104
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 81
- 229910052757 nitrogen Inorganic materials 0.000 description 52
- 230000018044 dehydration Effects 0.000 description 23
- 238000006297 dehydration reaction Methods 0.000 description 23
- 230000006837 decompression Effects 0.000 description 22
- 238000009413 insulation Methods 0.000 description 21
- 238000011049 filling Methods 0.000 description 15
- 238000003756 stirring Methods 0.000 description 15
- 238000004821 distillation Methods 0.000 description 14
- 238000003760 magnetic stirring Methods 0.000 description 14
- 229920001451 polypropylene glycol Polymers 0.000 description 14
- 238000010792 warming Methods 0.000 description 14
- 239000003292 glue Substances 0.000 description 11
- 238000001125 extrusion Methods 0.000 description 8
- 239000004588 polyurethane sealant Substances 0.000 description 8
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000004806 packaging method and process Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- GAPYKZAARZMMGP-UHFFFAOYSA-N pyridin-1-ium;acetate Chemical compound CC(O)=O.C1=CC=NC=C1 GAPYKZAARZMMGP-UHFFFAOYSA-N 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- AKCRQHGQIJBRMN-UHFFFAOYSA-N 2-chloroaniline Chemical compound NC1=CC=CC=C1Cl AKCRQHGQIJBRMN-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C11/00—Details of pavings
- E01C11/02—Arrangement or construction of joints; Methods of making joints; Packing for joints
- E01C11/04—Arrangement or construction of joints; Methods of making joints; Packing for joints for cement concrete paving
- E01C11/10—Packing of plastic or elastic materials, e.g. wood, resin
-
- 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
- C08L2312/00—Crosslinking
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Sealing Material Composition (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a moisture-curable self-cross-linked cement concrete pavement joint sealant. Silicon hydroxyl is used for substituting an isocyanate group to perform the cross-linking curing. The joint sealant is one-component, when in use, as long as the joint sealant is extruded, the component in the joint sealant can react with water in the air to be cured in a cross-linking manner; and the joint sealant is a novel polyurethane prepolymer formed by synthesizing polyether polyol, isocyanate, end hydroxyl organic silicon, a methoxyl end-capped hyperbranched polymer, a catalyst, a cross-linking agent and pigments. The moisture-curable self-cross-linked cement concrete pavement joint sealant solves the problems that the traditional joint sealant is afraid of water when in construction operation and utilizes carcinogenic cross-linking agent MOCA, still maintains the characteristics of good cohesiveness, embedding resistance and aging resistance, and is a novel polyurethane joint sealant which is long in shelf life, relatively environment-friendly and capable of well solving the influence of uncertain factors such as weather on the joint sealing operation progress of a cement pavement.
Description
The present invention relates to cement pavement pointing field, particularly to a kind of organic silicon modified polyurethane gap-filling glue containing hyperbranched polyamine-ester, and the preparation method of described organic silicon modified polyurethane gap-filling glue.
Background technology
The most frequently used cement pavement gap-filling glue of current China is based on polyurethane sealant, it is with the watertight of its excellence, air-tightness, high resiliency, caking property and durable, weatherability etc., can be long-term through Tensile, compression and vibration, cohesive force is strong, be amenable to seam crossing expand with heat and contract with cold repeatedly stretch, compression and the advantage such as destroyed and construction method is convenient, it is widely used in cement concrete pavement, the quality making cement concrete pavement is improved, and service life of road surface is effectively extended simultaneously.
Polyurethane sealant is to be polymerized by isocyanates and polyether polyol, generally has one-component and double-component two kinds.Containing highly polar groups such as-NCO and-OH in polyurethane filling material molecular structure, reaction can form tough elastic bonding layer after solidifying.Polyurethane sealant has the feature such as oil resistant, wear-resisting, vibration resistance, endurance, high-low temperature resistant simultaneously.The existing organic silicon modified polyurethane gap-filling glue method by introducing silicone segments in molecule, it is poor that the introducing of siliconoxygen bond solves traditional polyurethane filling material weatherability, under long-term sunlight irradiates, it is easy to the shortcomings such as efflorescence turns yellow, shortening in service life.
But, be traditional polyurethane sealant or organic-silicon-modified after polyurethane sealant all be by-NCO crosslinking, and-NCO is as easy as rolling off a log and active hydrogen reaction, when there being water to exist, this isocyanate terminated polyurethane prepolymer is known from experience solidification and is discharged carbon dioxide, making glue-line bubble, this has had a strong impact on the service life of polyurethane filling material, especially affects its construction under misty rain weather condition.Additionally, isocyanate terminated polyurethane sealant uses the double; two o-chloraniline (MOCA) of methine as cross-linking agent, this material is identified has carcinogenesis to human body.
At present, some developed countries are devoted to study a kind of novel cross-linking agent on the one hand in the world, it is intended to replace MOCA；It is also dedicated on the other hand study a kind of waterproof polyurethane sealant.Thus it is necessary a kind of novel pointing replacing traditional isocyanate terminated crosslinking curing of research and development, do not need again MOCA as cross-linking agent simultaneously.
Dissaving polymer space structure presents spherical, there is the structure that comparison is regular, end contains substantial amounts of active group, its highly branched structure imparts dissaving polymer high reaction activity, the features such as low viscosity, therefore can pass through the functional end-group to dissaving polymer modified thus obtaining the modified ultra-branching polymer of differential responses demand.Current dissaving polymer all embodies huge using value in fields such as coating, binding agent, biomaterial, drug carrier.
Summary of the invention
The problem water funk in order to solve traditional isocyanate terminated base polyurethane prepolymer for use as, the invention provides a kind of moisturecuring self-crosslinking, and there is good high-low temperature resistant, caking property, the feature such as ageing-resistant, and there are good anti-embeddability and elastomeric Joint Sealants for Cemcent Concrete Pavement.
Present invention also offers the described preparation method containing hyperbranched organic silicon modified polyurethane gap-filling glue.
Described cement concrete pavement pointing, the preparation technology of its base polyurethane prepolymer for use as is as follows:
Polyether polyol is joined in the reaction vessel of dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise MDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
Existing industrial production polyurethane sealant is generally adopted by prepolymer method, it is obtained by reacting isocyanate-terminated base polyurethane prepolymer for use as by isocyanates and polyether polyol, but-NCO very easily with active hydrogen reaction, glue-line so can be caused to bubble, shortening the service life of gap-filling glue, this has resulted in the difficulty in the construction of misty rain weather.It is contemplated that with the base polyurethane prepolymer for use as of Si-OH end-blocking, when methoxyl group makees cross-linking agent, add catalyst, so just can react with water when there being water to exist, crosslinking curing, thoroughly solve its water funk problem.
First pass through the base polyurethane prepolymer for use as of the consumption synthesizing isocyanate base end-blocking regulating polyether polyol and MDI, again through the base polyurethane prepolymer for use as of the consumption synthesis silicone hydroxyl end-blocking of the content of-NCO in mensuration system and the hydroxyl-terminated injecting two methyl siloxane of addition, this base polyurethane prepolymer for use as is, by under the Si-OH of end and the combined effect of cross-linking agent and catalyst, crosslinking curing occurs.
Utilizing some performances of dissaving polymer, as dissolubility is good, viscosity is low, and end can be used to modifiy with substantial amounts of active group and obtains the group that we want.Building-up process is simple, it is not necessary to separating-purifying, and production cost is low, and therefore the present invention wants to synthesize the dissaving polymer cross-linking agent as this product that a kind of end contains a large amount of methoxyl group.
The preparation of dissaving polymer:
(1) joining in the there-necked flask with magnetic stirring apparatus by diethanolamine and methanol, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, passes into nitrogen, open magnetic stirring apparatus in the middle of there-necked flask so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer, reaction equation is as follows:
(2) adding trimethylolpropane in above-mentioned system as core molecule, p-methyl benzenesulfonic acid, as catalyst, passes into nitrogen, stirs and be all completely dissolved to solid under the atmosphere of nitrogen protection, is then warming up to 85 DEG C, insulation reaction 24h, and reaction equation is as follows:
It is 396-566mgKOH/g by adopting the hydroxyl value that acetic acid pyridine circumfluence method determines synthesized dissaving polymer.From the mensuration of hydroxyl value, synthesized dissaving polymer end contains substantial amounts of hydroxyl.
Adding 3-NCO propyl trimethoxy silicane in above-mentioned reaction system, maintain the temperature at about 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group, and it is as follows that reaction terminates rear structural formula
It is 9-31mgKOH/g by adopting the hydroxyl value that acetic acid pyridine circumfluence method determines synthesized dissaving polymer.From the mensuration of hydroxyl value, the synthesized substantial amounts of hydroxyl of dissaving polymer end disappears, and illustrates that our modification ratio is more successful.
The performance test of the Joint Sealants for Cemcent Concrete Pavement of the present invention
The product extrusion that will obtain, in atmosphere after full cross-linked solidification, carrying out performance test, its surface drying time is at 7h, and needle penetration is 3.8mm, elastic restoration ratio 78%, hot strength is 0.66MPa, and adhesion strength is 0.48MPa, and elongation at break is 432%, 80 DEG C of * 168h of high temperature do not trickle, and-40 DEG C of * 168h of low temperature do not rupture.Cement pavement is because of four seasons alternate, the temperature difference is bigger, cement sheeting can produce the phenomenon that hot pressing is cold drawn, therefore at-30 DEG C and 20 DEG C, this gap-filling glue carried out the cold drawn experiment of hot pressing, experiment proves that this pointing is possible not only to carry out at 100% time, and displacement remains to reach the requirement of 50% over numerous cycles, and adhesion strength can reach 0.33MPa, has all reached Standard.
The invention has the beneficial effects as follows:
The present invention this containing hyperbranched organic silicon modified polyurethane pointing under overcoming the tradition water funk premise of gap-filling glue, can directly react with water, moisturecuring self-crosslinking, and this product is single-component product, directly extrude during use to cement gap, easy to use, and to environment non-hazardous, safety and environmental protection.This pointing still maintains the characteristics such as good resistant of high or low temperature, anti-embeddability and caking property on this basis, is a kind of long service life, and the novel pointing that cost is low has good market prospect.
Embodiment
The following is the statement that specific implementation method of the present invention is more detailed, it is therefore intended that set forth design and the feature of the present invention, can not limit the scope of the invention with this.All equivalences made according to spirit of the invention change or modify, and all should be encompassed within protection scope of the present invention.
Hereinafter the cement pavement pointing of the present invention is described in more detail, its object is to illustrate to limit the scope of the invention design and the feature of the present invention with this.All equivalences made according to spirit of the invention change or modify, and all should be encompassed within protection scope of the present invention.
Embodiment one
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 6.7g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 3g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 35g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Embodiment two
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 2.2g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 3g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 35g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Embodiment three
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 1.0g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 3g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 35g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Embodiment four
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 2.2g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 5g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 35g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Embodiment five
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 2.2g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 2g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 35g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Embodiment six
(1) precise 16g(0.15mol) diethanolamine, 13g(0.15mol) acrylic acid methyl ester. and 75ml methanol, first diethanolamine and methanol are joined in the there-necked flask with magnetic stirring apparatus, flask mouth is connected with 100 DEG C of thermometeies and Dropping funnel respectively, nitrogen is passed in the middle of there-necked flask, open magnetic stirring apparatus so that diethanolamine and methanol are fully miscible.Then being added in Dropping funnel by acrylic acid methyl ester., be added drop-wise in the middle of flask slowly, after dropwising, heating in water bath is warming up to 40 DEG C, and the product being obtained by reacting then is transferred in the middle of Rotary Evaporators by insulation reaction 6h, and reduce pressure distillation for removing methanol, obtains AB2Type monomer.
(2) in above-mentioned system, 6.7g(0.05mol is added) trimethylolpropane is as core molecule; adding mass fraction is that the p-methyl benzenesulfonic acid of 0.5% is as catalyst; pass into nitrogen; stir under the atmosphere of nitrogen protection and be all completely dissolved to solid, be then warming up to 85 DEG C, insulation reaction 24h; 60g(0.3mol is added in reaction system) 3-NCO propyl trimethoxy silicane; at 85 DEG C, insulation reaction 6h, decompression distillation has just been prepared end and has been contained the dissaving polymer of a large amount of methoxyl group.
(3) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(4) 3g(2 is taken) the middle dissaving polymer synthesized, and amount to the following filler of 25g, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst join in (3) that reaction terminates, at a certain temperature, high-speed stirred is uniform, it is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recover normal pressure, close vacuum system, pack with extruder discharging.
(5) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Comparison example
(1) being 2000 by 15g molecular weight, hydroxyl value is 54-57mgOH/g polyoxypropyleneglycol, and 10g molecular weight is 3000, and hydroxyl value is in the reaction vessel that 56-58mgOH/g polypropylene oxide triol joins dry cleansing.Under the vacuum of about-0.092MP, open circulating condensing water, open stirring, control temperature at about 90 DEG C, dehydration until on condenser substantially anhydrous out time, be cooled to 50 DEG C.Under nitrogen protection, being slowly added dropwise 6.9gMDI in above-mentioned system, the strict reaction temperature that controls, about the 50 DEG C generations preventing implode from reacting, dropwises in 30min, is then to slowly warm up to 85 DEG C (± 2 DEG C), polymerization under atmospheric pressure reaction 2h.Then dripping 17.5g molecular weight in system is the hydroxyl-terminated injecting two methyl siloxane of 1000, after reaction 3h, close nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, it is then shut off vacuum system, open nitrogen intake valve, make system recover normal pressure.It is cooled to 70 DEG C.
(2) the following filler of 35g altogether is taken, Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst and MTMS join in (1) that reaction terminates, at a certain temperature, high-speed stirred is uniform, is then shut off nitrogen intake valve, open vacuum system, maintain temperature when 85 DEG C (± 2 DEG C) and vacuum about-0.092MP, decompression dehydration 2-3h, then recovers normal pressure, close vacuum system, pack with extruder discharging.
(3) when using, opening packaging, be directly filled in the gap of cement concrete pavement by filler extrusion, the end group in pointing can solidify by self-crosslinking at normal temperatures with the water in air.
Performance detects
The polyurethane filling material of examples detailed above is carried out performance test, and it is as shown in the table for its result:
| Elongation at break % | Hot strength MPa | Adhesion strength MPa | Needle penetration mm | Hot pressing-cold drawn circulation MPa | High temperature resistant 80 DEG C | Low temperature resistant-40 DEG C | |
| Embodiment one | 415 | 1.03 | 0.6 | 2.6 | 0.54 | Do not trickle | Do not rupture |
| Embodiment two | 468 | 0.88 | 0.58 | 3.4 | 0.53 | Do not trickle | Do not rupture |
| Embodiment three | 422 | 0.79 | 0.45 | 4.2 | 0.42 | Do not trickle | Do not rupture |
| Embodiment four | 433 | 0.81 | 0.62 | 3.0 | 0.45 | Do not trickle | Do not rupture |
| Embodiment five | 437 | 0.76 | 0.55 | 3.7 | 0.42 | Do not trickle | Do not rupture |
| Embodiment six | 483 | 0.83 | 0.54 | 4.4 | 0.38 | Do not trickle | Do not rupture |
| Comparison example | 432 | 0.66 | 0.48 | 3.8 | 0.43 | Do not trickle | Do not rupture |
Note: above testing standard adopts JT/T589-2004.
Be can be seen that by data in table, add after dissaving polymer the performances such as the hot strength of product, elongation at break, adhesion strength to be improved, and institute's test performance result is above national standard requirement, and based on the increase of various fillers, its cost is also below market product, and solves the shortcoming that conventional urethane gap-filling glue is water funk, this product only need to be extruded in use and expose the product in air, it is made to react with the water in air, crosslinking curing, easy to use.Illustrate that what the present invention synthesized is the pointing of a kind of desirable novel environment friendly containing hyperbranched organic silicon modified polyurethane gap-filling glue.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention also should not be limited by the examples; the change made under other any spirit without departing from the present invention and principle, modification, combination, replacement, simplification all should be equivalence substitute mode, are included within protection scope of the present invention.
Claims (9)
1. the Joint Sealants for Cemcent Concrete Pavement of a moisturecuring self-crosslinking, it is characterized in that one-component, this product is obtained base polyurethane prepolymer for use as by polyether polyol and isocyanate polymeric, the base polyurethane prepolymer for use as of silicone hydroxyl end-blocking it is obtained by reacting again with hydroxyl-terminated injecting two methyl siloxane, then the dissaving polymer containing a large amount of methoxyl group with end is crosslinking curing under having water existent condition, and the end of described dissaving polymer is methoxyl group；
The hydroxy number of NCO and polyether polyol is than for 2.2:1；
Hydroxyl-terminated injecting two methyl siloxane terminal hydroxyl terminate with preliminary polymerization after NCO number than for 1.8:1；
The weight ratio of the dissaving polymer of end silicone hydroxyl base polyurethane prepolymer for use as and methoxy group is 20:1.
2. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterized in that the weight ratio of end silicone hydroxyl base polyurethane prepolymer for use as, cross-linking agent and filler is 20:1:7, filler is more than one in Pulvis Talci, precipitated calcium carbonate, aerosil, pigment, plasticizer, catalyst.
3. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that cross-linking agent is the dissaving polymer of synthesized methoxy group.
4. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that the hydroxyl value of polyether polyol is 54-58mgKOH/g.
5. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that its end group of the dissaving polymer of synthesis is methoxyl group.
6. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that dissaving polymer is prepared by following method:
16g diethanolamine, 13g acrylic acid methyl ester. are obtained by reacting AB2Type monomer, add 2.2g trimethylolpropane as core molecule, add the p-methyl benzenesulfonic acid that mass fraction is 0.5% and obtain Hyperbranched Polymer with Terminal Hydroxyl as catalyst reaction, then be modified obtaining end methoxyl group dissaving polymer to Hyperbranched Polymer with Terminal Hydroxyl with 60g3-NCO propyl trimethoxy silicane.
7. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterized in that directly being expressed in cement pavement gap when using, the base polyurethane prepolymer for use as of silicone hydroxyl end-blocking and methoxyl group meeting quickly crosslinking curing under having water existent condition in product, this process is simple and easy to operate, and Environmental Safety.
8. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that trimethylolpropane and 3-NCO propyl trimethoxy silicane mol ratio are 1:3,1:9 or 1:21.
9. Joint Sealants for Cemcent Concrete Pavement according to claim 1, it is characterised in that when dissaving polymer uses as cross-linking agent, dosage is the 2%-5% of the base polyurethane prepolymer for use as of silicone hydroxyl end-blocking.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610175923.XA CN105733490B (en) | 2016-03-25 | 2016-03-25 | A kind of cement concrete pavement gap-filling glue of moisturecuring self-crosslinking |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610175923.XA CN105733490B (en) | 2016-03-25 | 2016-03-25 | A kind of cement concrete pavement gap-filling glue of moisturecuring self-crosslinking |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105733490A true CN105733490A (en) | 2016-07-06 |
| CN105733490B CN105733490B (en) | 2018-05-04 |
Family
ID=56251494
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610175923.XA Active CN105733490B (en) | 2016-03-25 | 2016-03-25 | A kind of cement concrete pavement gap-filling glue of moisturecuring self-crosslinking |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105733490B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200849A (en) * | 2017-05-17 | 2017-09-26 | 江苏超力建材科技有限公司 | A kind of cement road seam aqueous interfacial agents and its preparation method and application |
| CN108384024A (en) * | 2018-03-19 | 2018-08-10 | 济南大学 | A kind of preparation improving self-adhesive asphalt waterproof coiled material adhesive property hyperbranched resin |
| CN110257001A (en) * | 2019-07-15 | 2019-09-20 | 江苏盛世海新材料科技有限公司 | A kind of flexibility joint trimming agent |
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
| CN111218876A (en) * | 2018-11-27 | 2020-06-02 | 长春市市政工程设计研究院 | Cement concrete pavement wet assembling process with three-dimensional embedding and extruding joint |
| CN118006280A (en) * | 2024-04-08 | 2024-05-10 | 山东广亚新材料有限公司 | Organosilicon modified polyurethane sealant |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5578406B2 (en) * | 2009-11-25 | 2014-08-27 | 旭化成ホームズ株式会社 | One-part moisture curable sealant composition for improving antibacterial and antifungal properties of outer wall joint top coating film, and method for improving antibacterial and antifungal properties of outer wall joint top coating film using the same |
| CN102604368B (en) * | 2012-03-02 | 2013-09-11 | 江苏超力建材科技有限公司 | NCO replaced crosslinking cured joint filling material for concrete pavement |
| CN202766943U (en) * | 2012-09-24 | 2013-03-06 | 河南万里路桥集团有限公司 | Filling and sealing structure for cement concrete pavement slit |
| CN103408924B (en) * | 2013-07-10 | 2015-08-19 | 万铜岭 | Joint closure material |
| CN103756289B (en) * | 2013-12-20 | 2016-08-17 | 河南万里路桥集团有限公司 | Pavement crack cementation of fissures material and preparation method thereof |
-
2016
- 2016-03-25 CN CN201610175923.XA patent/CN105733490B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
| CN107200849A (en) * | 2017-05-17 | 2017-09-26 | 江苏超力建材科技有限公司 | A kind of cement road seam aqueous interfacial agents and its preparation method and application |
| CN107200849B (en) * | 2017-05-17 | 2020-06-09 | 江苏超力建材科技有限公司 | Water-based interface agent for cement highway joint and preparation method and application thereof |
| CN108384024A (en) * | 2018-03-19 | 2018-08-10 | 济南大学 | A kind of preparation improving self-adhesive asphalt waterproof coiled material adhesive property hyperbranched resin |
| CN111218876A (en) * | 2018-11-27 | 2020-06-02 | 长春市市政工程设计研究院 | Cement concrete pavement wet assembling process with three-dimensional embedding and extruding joint |
| CN110257001A (en) * | 2019-07-15 | 2019-09-20 | 江苏盛世海新材料科技有限公司 | A kind of flexibility joint trimming agent |
| CN118006280A (en) * | 2024-04-08 | 2024-05-10 | 山东广亚新材料有限公司 | Organosilicon modified polyurethane sealant |
| CN118006280B (en) * | 2024-04-08 | 2024-07-02 | 山东广亚新材料有限公司 | Organosilicon modified polyurethane sealant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105733490B (en) | 2018-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105733490A (en) | Moisture-curable self-cross-linked cement concrete pavement joint sealant | |
| CN102676039B (en) | Moisturecured one-component polyurethane paint and preparation method thereof | |
| CN102775900B (en) | Water curing asphalt polyurethane composite waterproof coating and preparation method thereof | |
| CN103992633B (en) | A kind of polyurethane caulking material for ballastless track of high-speed railway expansion joint | |
| CN102807812A (en) | Latent curing single-component polyurethane water-proof coating and preparation method thereof | |
| CN102816549B (en) | Silyl-terminated polyether modified polyurethane adhesive, its preparation method and application thereof | |
| CN109554101A (en) | A kind of polyurethane water-proof paint | |
| CN107216845A (en) | A kind of environment-friendly type end siloxy group polyurethane sealant and preparation method thereof | |
| CN102604368B (en) | NCO replaced crosslinking cured joint filling material for concrete pavement | |
| CN102140243A (en) | Plastic sizing agent for silane-modified single component wet cured polyurethane playing court and preparation method thereof | |
| CN105176474A (en) | Road crack-filling adhesive suitable for wet-surface crack and preparation method thereof | |
| CN102424721A (en) | Environment friendly plastic slurry for sports field and preparation method thereof | |
| CN106433439B (en) | A kind of cold uncured polyurethane water-proof paint and preparation method thereof of constructing | |
| US11566098B2 (en) | Graphene-modified elastomer material and its preparation method | |
| CN103131162B (en) | Specially-used enhanced polyurethane sealing water-stopping material and production method thereof | |
| CN104804699A (en) | Hot melt adhesive | |
| CN105419718A (en) | Preparation method for high-strength artificial turf polyurethane gum | |
| CN104262571A (en) | Preparation method and application of soft high-solid-content waterborne polyurethane resin | |
| CN112094581B (en) | Solvent-free fast-curing reactive waterproof coating and preparation method thereof, and coil coating superposed waterproof structural system and construction method thereof | |
| CN107739519A (en) | A kind of modified pitch of waterproof roll and preparation method thereof | |
| CN105199653B (en) | A kind of high intensity low viscosity silicane-modified polyurethane resin | |
| CN109321196A (en) | Anti-skid surface dual-component polyurethane adhesive and preparation method thereof | |
| CN104211902A (en) | Preparation method of waterborne polyurethane emulsion and waterborne polyurethane emulsion prepared by preparation method | |
| CN1326966C (en) | Organic silicon modified polyurethane gap-filling rubber for cement road | |
| CN107082866B (en) | Waterproof coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201216 Address after: 271000 west house, 2 / F, Tower B, Taishan science and Technology City, hi tech Zone, Tai'an City, Shandong Province Patentee after: SHANDONG BAOSHENG NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: Jinan University, no.336, nanxinzhuang West Road, Shizhong District, Jinan City, Shandong Province, 250022 Patentee before: University of Jinan |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A moisture cured self crosslinking cement concrete pavement sealant Granted publication date: 20180504 Pledgee: Taian Bank Co.,Ltd. Daizong sub branch Pledgor: SHANDONG BAOSHENG NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2024980016804 |