CN101805588A - Polyurethane road caulking sealant with good durability and production process - Google Patents
Polyurethane road caulking sealant with good durability and production process Download PDFInfo
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Abstract
The invention relates to polyurethane road caulking sealant with good durability and a production process. The polyurethane road caulking sealant comprises an ingredient A and an ingredient B, wherein the ingredient A is prepared through the reaction of low-unsaturation-degree high-molecular-weight polyether glycol, hydroxyl silicone oil and aliphatic isocyanate for a certain time at a certain temperature, and the ingredient B is prepared through grinding mixed materials for three times after uniformly mixing liquid polyurethane plasticizing agents, mixing liquid (prepared from tap water and surface active agents), filling materials, pigment and defoaming agents at normal temperature and under normal pressure. The ingredient A and the ingredient B are uniformly mixed according to a weight ratio of 1/2, and elastic sealant is obtained after the mixture is cured. Products conform to the requirements of the standard of Sealant for Road and Bridge Caulking JC/T 976-2005. The products have excellent durability, a service life of between 10 and 15 years, and can be widely applied to the caulking sealing of gaps of concrete highway, bridges, airfield runway, ballastless rail high-speed railway and the like. The polyurethane road caulking sealant belongs to a regeneration product of the existing ordinary polyurethane road caulking sealant.
Description
Technical field
The present invention relates to a kind of polyurethane road caulking sealant with good durability and production technique, this product have better weather-resistant performance than the general polyurethane road caulk compound that uses at present and the usage period longer, the filling sealing in slit such as can be widely used between concrete express way, bridge, airfield runway, agricultural irrigation channel, non-fragment orbit high-speed railway bridge bed-plate.Be generally working life 10～15 years.
Technical background
The elastic sealant that is used for the slit filling usefulness between concrete express way, bridge, airfield runway, non-fragment orbit high-speed railway bridge bed-plate at present mainly contains the polyurethane road caulk compound, gathers three kinds of sulphur road joint glue, silicone road joint glues.
Though silicone road joint glue ageing-resistant performance, excellent heat resistance also have some shortcomings: it has good cohesiveness for building materials such as glass or metal aluminiums, but for the then difficult relatively bonding of concrete material.Reason mainly is because the alkalescence of cement concrete own is very strong, can destroy the chemical hydrolysis bonding of bonding interface; Next is that cement concrete surface is loose porous, moisture-sensitive moisture absorption, influence bonding.In addition to concrete easily corrode, oil impregnate pollutes (softening agent move out easily surface), easily defective such as tears, problem is more outstanding in the waterproof sealing of structural joints such as concrete prefabricated board and stone material body of wall seam, airport, bridge concrete and glass fiber reinforced concrete especially, and price is more expensive, and therefore overall consumption is little.
That the polyurethane road caulk compound has is strong with concrete binding power, good-extensibility, wear-resisting anti-puncture, base material is not polluted, acid and alkali-resistance, organic solvent-resistant, stone material and concrete are not had burn into is suitable for characteristics such as dynamic adhesion, it is ageing-resistant, resistance toheat is poorer slightly than silicone road joint glue, and be 3～5 years general working life.Because of its moderate cost, its widely-used favourable condition that provides in civil construction is provided for this.
The polyurethane road caulk compound uses at present single component and two-pack, and single component requires packing strict, and the moisture absorption easily, and the quality guaranteed period is short, and complex manufacturing will adopt vacuum duplicate rows star kneader to mix, and price comparison is expensive.And two-pack adopts the separately form of packing, to packing, production requirement is not very strict, long, price of shelf lives compared with single component will be low many, competitive edge is obvious, therefore is used at present the still two component polyurethane road joint glue that fill in the slit between concrete express way, bridge, airfield runway, non-fragment orbit high-speed railway bridge bed-plate in a large number.
Poly-sulphur road joint glue has that oil-proofness is good, high and low temperature resistance is good, uses more at airport hardstand.But the UV resistant performance is not so good, though it is better to use the initial stage over-all properties, after 1～2 year, cracking, hardening phenomenon will occur, makes seal failure, needs to repair and the cementation of fissures again.
Because concrete express way, bridge, airfield runway, non-fragment orbit high-speed railway need reduce maintenance, though and at present general polyurethane road caulk compound is moderate, but ageing-resistant, wet-hot aging performance is relatively poor, safeguards frequently, expends lot of manpower and material resources.Therefore develop that a kind of ageing-resistant performance is superior, the rational polyurethane road caulk compound of cost performance, will there be huge economic benefit and social benefit the usage period 10～15 years (according to external service conditions such as the U.S., Japan).
Summary of the invention
Adopt polyether polyalcohol with low unsaturation degree and high molecular weight, hydroxy silicon oil and aliphatic isocyanates at 85～90 ℃ according to above-mentioned technical background this patent, reaction 2～3h obtains base polyurethane prepolymer for use as, as the product A component.Liquid polyurethane softening agent, mixed solution (water, surfactant mixtures), filler, pigment, defoamer are mixed, grind three times, as the product B component.A, B are even according to the mixed of 1: 2 (weight ratio), and the water in the B component is done to become elastic sealant after solidifying agent solidifies.Product meets " bridge filleting seal gum " JC/T 976-2005 standard-required.
Polyether polyalcohol with low unsaturation degree and high molecular weight is a dibasic alcohol, M
n=5000～12000.
Hydroxy silicon oil is the end capped polydimethylsiloxane of low-molecular-weight hydroxyl, and molecular formula is HO-[S
i(CH
3)
2-O-]
n-H is polymerization degree n=4～11 wherein.
Aliphatic isocyanates is isophorone diisocyanate (IPDI), hexamethylene-diisocyanate HDI and trimer thereof etc.
Polyether glycol in the liquid polyurethane softening agent is N204, N210, lower molecular weights such as N220 two functional group's polyether glycols, isocyanic ester are isophorone diisocyanate (IPDI), hexamethylene-diisocyanate HDI and trimer thereof, TDI, MDI or modification MDI etc.Alcohol is the alcohol of single functionality, as propyl carbinol, Pentyl alcohol, n-hexyl alcohol etc.
Mixed solution is water, surfactant mixture.Water wherein: tensio-active agent=1: 0.1～0.2.. the surface treatment agent in the mixed solution is nonionogenic tenside or anion surfactant, and water is clean tap water.
Filler is flyash, talcum powder, water-ground limestone, light calcium carbonate, nano modification water-ground limestone, aerosil, antioxidant 1010, UV-327 UV light absorber etc.
Pigment is iron oxide red, carbon black etc.
Auxiliary agent is a defoamer, is fine calcium oxide etc.
The production technique of superior durability polyurethane road caulk compound is:
1) in the interlayer enamel reaction still, add polyether polyalcohol with low unsaturation degree and high molecular weight, hydroxy silicon oil by proportioning earlier, in temperature is 105～110 ℃, and the 2h that dewaters under the condition of vacuum tightness for-0.086MPa is cooled to 60 ℃, add aliphatic isocyanates, continue to be warming up to 85～95 ℃, reaction 2～3h obtains base polyurethane prepolymer for use as, be cooled to below 50 ℃, be packaged to be the A component.
2) in the interlayer enamel reaction still, add polyether glycol by proportioning earlier, in temperature is 105～110 ℃, vacuum tightness is-and the 0.086MPa 2h that dewaters, be cooled to 60 ℃, add isocyanic ester, continue to be warming up to 75～80 ℃, reaction 3～4h adds alcohol again, reaction 2h is cooled to 50 ℃ and obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add liquid polyurethane softening agent, mixed solution, filler, pigment, auxiliary agent etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
Production technology characteristic: the B component at normal temperatures and pressures with water as linking agent, the MOCA solidifying agent of abandoning tradition, it needs high-temperature digestion to go in the B component, the technology more complicated.Though also have liquid MOCA to sell at present, price is than solid MOCA expensive (though solid MOCA is also more expensive).In addition, MOCA finds to have carcinogenic suspicion, has been limited to use in some countries, and by other more material replacement of environmental protection, but price is all more expensive.And adopt tap water to make solidifying agent, environmental protection more economically will seem.
By a kind of polyurethane road caulking sealant with good durability of prescription disclosed by the invention and explained hereafter, after testing, the basic mechanical design feature index meets " bridge filleting seal gum " JC/T 976-2005 standard-required.See Table 1.
Table 1 " bridge filleting seal gum " JC/T 976-2005 standard
| Test subject | Technical indicator |
| Outward appearance | Fine and smooth, even thickness body/body of paste |
| Test subject | Technical indicator |
| Mobile (S type) | Smooth smooth |
| Surface drying time, h | ??≤8 |
| Elastic restoration ratio, % | ??≥70 |
| Tensile modulus, MPa, 23 ℃ | ??≤0.4 |
| Surely stretch cohesiveness | Do not have and destroy |
| Surely stretch cohesiveness after the immersion | Do not have and destroy |
| Mass loss, % | ??≤8 |
Product is constructed at normal temperatures, and according to the A component: the B component=ratio stirred in 1: 2, it is poured in the slit go by scraper, applicator gun, other encapsulating instrument.It is longer that it has superior weather-resistant performance and a usage period than present general polyurethane road caulk compound, can be widely used between concrete express way, bridge, airfield runway, agricultural irrigation channel, non-fragment orbit high-speed railway bridge bed-plate etc. the slit the filling sealing.Be generally working life 10～15 years.
The principle of polyurethane road caulking sealant with good durability is according to being:
(1) employing has hydroxy silicon oil, polyether polyalcohol with low unsaturation degree and high molecular weight and aliphatic isocyanates reaction, to improve its ageing-resistant performance.
1 hydroxy silicon oil is a kind of hydroxy-end capped polysiloxane, is a kind of superior structural control agent commonly used in the silastic product industry.
Structural formula
Owing to its particular structure has fabulous high and low temperature resistance, excellent chemical stability etc.Therefore, in the preparation process of polyurethane road caulk compound, add a certain amount of hydroxy silicon oil, the silica (S of formation
i-O) key is inserted in the main chain of urethane and goes, and since the bond energy higher (422.5KJ/mol) of siloxane bond, the bond angle broad, and therefore heat-resisting, ageing resistance is the good of main chain than general carbon-to-carbon, carbon-oxygen, nitrogen-hydrogen bond.The advantage separately of two kinds of structural units of performance like this helps further to improve that material is weather-proof, water-fast, resistant to chemical media, anti-fuel oil and characteristic such as heat-resisting.
2 polyether glycols be produce the polyurethane road caulk compound main raw material, but common polyether glycol degree of unsaturation is big.Residual unsaturated link(age) in the polyurethane road caulk compound that it makes is subjected to effects such as daylight, temperature, moisture can be oxidized to aldehyde ketone and carboxylic acid gradually, and further catalysis causes the material aging degraded, produces the xanthochromia group, thereby makes the resistant polyurethane ultraviolet ray poor.And the polyether polyalcohol with low unsaturation degree and high molecular weight degree of unsaturation is extremely low, can prevent because of two keys oxidizedly, makes it have splendid weathering resistance.
3 usual to produce the polyurethane road caulk compounds mainly be TDI, MDI or its mixture, and when being subjected to the influencing of factor such as photo-thermal when it, the benzene nucleus of TDI, MDI progressively is oxidized to quinone structure, and this structure causes the urethane flavescence.Ammonia ester bond in the aliphatic isocyanates is stable than the ammonia ester bond of aromatic isocyanate, even resolve into aliphatic amide, also is difficult for oxidizedly, so ageing resistance is superior.
(2) adopt homemade polyurethane plasticizer to substitute traditional DBP, DOP softening agent (country must not stipulate artificially add), increase material compatibility, also improved ageing-resistant performance.
The basic raw material of preparation polyurethane plasticizer mainly is alcohol compound and isocyanic ester.With the elastomeric difference of synthesis of polyurethane be the synthetic single functionality alcohol or the single functionality isocyanic ester of needing of polyurethane plasticizer.The adding the inertia (anergy group) that the people guaranteed polyurethane plasticizer and keep liquid suitable molecular weight of single functionality material.Characteristic is 1) with base polyurethane prepolymer for use as good intermiscibility is arranged, non-volatile, do not move.2) plasticising mechanism uniqueness, plasticising goods good endurance.It is generally acknowledged. the plasticising mechanism of softening agent is that the superpolymer free volume changes the segment that originally can't move in body can be moved, thereby plays plastification because the adding of softening agent causes macromolecular chain to ask that interaction weakens.Softening agent such as DOP commonly used, DBP etc. can improve the elasticity of polymer materials, winter hardiness and shock strength, but the thermotolerance of material and tensile strength and ageing-resistant performance reduce when using polyurethane plasticizer, except improving elasticity, outside winter hardiness and the shock strength. be improved on the contrary in certain amount ranges in-draw intensity, and to the not influence of material aging performance.This is that the mechanism of action of polyurethane plasticizer has its singularity.
Because softening agent such as DOP commonly used, DBP has easy migrate attribute, and people's reproductive function is had detrimental effect, and country must not stipulate and artificially adds at JC 1066-2008 " limits of harmful substances in the building water-proof paint ".
Specific embodiments
Embodiment one
1) in the interlayer enamel reaction still, adds 56% M earlier
n=5000 polyether polyalcohol with low unsaturation degree and high molecular weight, 20% n=6 hydroxy silicon oil, through 105～110 ℃ ,-0.086MPa the 2h that dewaters is cooled to 60 ℃, adds 24%HDI, is warming up to 85～90 ℃, and reaction 2～3h is cooled to packing below 50 ℃.Obtain base polyurethane prepolymer for use as, be packaged to be the A component.
2) in the interlayer enamel reaction still, add earlier 65.2% N210 polyether glycol, through 105～110 ℃ ,-0.086MPa the 2h that dewaters, be cooled to 60 ℃, the TDI of adding 24.3% is warming up to 75～80 ℃, reaction 3～4h, add 10.5% propyl carbinol again, reaction 2h is cooled to packing below 50 ℃, obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add 45% liquid polyurethane softening agent, 8% mixed solution, 43% filler, 3% pigment, 1% auxiliary agent etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
According to the A component: B component=1: 2 preparation sample.After testing, the basic mechanical design feature index sees Table 2.Meet " bridge filleting seal gum " JC/T 976-2005 standard-required.
Table 2 polyurethane road caulk compound basic mechanical design feature index
| Test subject | Technical indicator |
| Outward appearance | Fine and smooth, even thickness body |
| Mobile (S type) | Smooth smooth |
| Test subject | Technical indicator |
| Surface drying time, h | ??1.5 |
| Elastic restoration ratio, % | ??95 |
| Tensile modulus, MPa, 23 ℃ | ??0.38 |
| Surely stretch cohesiveness | Do not have and destroy |
| Surely stretch cohesiveness after the immersion | Do not have and destroy |
| Mass loss, % | ??2.5 |
Embodiment two
1) in the interlayer enamel reaction still, adds 68% M earlier
n=5000 polyether polyalcohol with low unsaturation degree and high molecular weight, 10% n=6 hydroxy silicon oil, through 105～110 ℃ ,-0.086MPa the 2h that dewaters is cooled to 60 ℃, adds 22%HDI, is warming up to 85～90 ℃, and reaction 2～3h is cooled to packing below 50 ℃.Obtain base polyurethane prepolymer for use as, be packaged to be the A component.
2) in the interlayer enamel reaction still, add earlier 65.2% N210 polyether glycol, through 105～110 ℃ ,-0.086MPa the 2h that dewaters, be cooled to 60 ℃, the TDI isocyanic ester of adding 24.3% is warming up to 75～80 ℃, reaction 3～4h, add 10.5% propyl carbinol again, reaction 2h is cooled to packing below 50 ℃, obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add 45% liquid polyurethane softening agent, 14% mixed solution, 37% filler, 3% carbon black, fine calcium oxide of 1% etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
According to the A component: B component=1: 2 preparation sample.After testing, the basic mechanical design feature index sees Table 3, meets " bridge filleting seal gum " JC/T 976-2005 standard-required.
Table 3 polyurethane road caulk compound basic mechanical design feature index
| Test subject | Technical indicator |
| Outward appearance | Fine and smooth, even thickness body |
| Mobile (S type) | Smooth smooth |
| Surface drying time, h | ??3.0 |
| Elastic restoration ratio, % | ??88 |
| Tensile modulus, MPa, 23 ℃ | ??0.32 |
| Test subject | Technical indicator |
| Surely stretch cohesiveness | Do not have and destroy |
| Surely stretch cohesiveness after the immersion | Do not have and destroy |
| Mass loss, % | ??4.7 |
Embodiment three
1) in the interlayer enamel reaction still, adds 56% M earlier
n=8000 polyether polyalcohol with low unsaturation degree and high molecular weight, 20% n=9 hydroxy silicon oil, through 105～110 ℃ ,-0.086MPa the 2h that dewaters is cooled to 60 ℃, adds 24%HDI, is warming up to 85～90 ℃, and reaction 2～3h is cooled to packing below 50 ℃.Obtain base polyurethane prepolymer for use as, be packaged to be the A component.
2) in the interlayer enamel reaction still, add earlier 65.2% N210 polyether glycol, through 105～110 ℃ ,-0.086MPa the 2h that dewaters, be cooled to 60 ℃, the TDI of adding 24.3% is warming up to 75～80 ℃, reaction 3～4h, add 10.5% propyl carbinol again, reaction 2h is cooled to packing below 50 ℃, obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add 60% liquid polyurethane softening agent, 8% mixed solution, 26% filler, 3% carbon black, 1% fine calcium oxide etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
According to the A component: B component=1: 2 preparation sample.After testing, basic mechanical design feature index table 4 meets " bridge filleting seal gum " JC/T 976-2005 standard-required.
Table 4 polyurethane road caulk compound basic mechanical design feature index
| Test subject | Technical indicator |
| Outward appearance | Fine and smooth, even thickness body |
| Mobile (S type) | Smooth smooth |
| Surface drying time, h | ??6.2 |
| Elastic restoration ratio, % | ??85 |
| Tensile modulus, MPa, 23 ℃ | ??0.25 |
| Surely stretch cohesiveness | Do not have and destroy |
| Surely stretch cohesiveness after the immersion | Do not have and destroy |
| Mass loss, % | ??3.2 |
Embodiment four
1) in the interlayer enamel reaction still, adds 68% M earlier
n=8000 polyether polyalcohol with low unsaturation degree and high molecular weight, 10% n=9 hydroxy silicon oil, through 105～110 ℃ ,-0.086MPa the 2h that dewaters is cooled to 60 ℃, adds 22%HDI, is warming up to 85～90 ℃, and reaction 2～3h is cooled to packing below 50 ℃.Obtain base polyurethane prepolymer for use as, be packaged to be the A component.
2) in the interlayer enamel reaction still, add earlier 65.2% N210 polyether glycol, through 105～110 ℃ ,-0.086MPa the 2h that dewaters, be cooled to 60 ℃, the TDI of adding 24.3% is warming up to 75～80 ℃, reaction 3～4h, add 10.5% propyl carbinol again, reaction 2h is cooled to packing below 50 ℃, obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add 60% liquid polyurethane softening agent, 14% mixed solution, 22% filler, 3% carbon black, 1% fine calcium oxide etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
According to the A component: B component=1: 2 preparation sample.After testing, the basic mechanical design feature index sees Table 5, meets " bridge filleting seal gum " JC/T 976-2005 standard-required.
Table 5 polyurethane road caulk compound basic mechanical design feature index
| Test subject | Technical indicator |
| Outward appearance | Fine and smooth, even thickness body |
| Mobile (S type) | Smooth smooth |
| Surface drying time, h | ??7.5 |
| Elastic restoration ratio, % | ??80 |
| Tensile modulus, MPa, 23 ℃ | ??0.20 |
| Surely stretch cohesiveness | Do not have and destroy |
| Surely stretch cohesiveness after the immersion | Do not have and destroy |
| Mass loss, % | ??5.2 |
Claims (8)
1. polyurethane road caulking sealant with good durability, it is characterized in that this caulk compound comprises A component and B component, wherein the weight proportion of A component is: polyether polyalcohol with low unsaturation degree and high molecular weight 50～70%, hydroxy silicon oil 5～25%, aliphatic isocyanates 15～30%.The weight ratio of B component is: liquid polyurethane softening agent 40～60%, mixed solution 5～15%, filler 20～40%, pigment 1～5%, auxiliary agent 0.5～1%.
The production technique of A component and B component is as described below:
1) in the interlayer enamel reaction still, earlier add polyether polyalcohol with low unsaturation degree and high molecular weight, hydroxy silicon oil successively by proportioning, in temperature is 105～110 ℃, and the 2h that dewaters under the condition of vacuum tightness for-0.086MPa is cooled to 60 ℃, add aliphatic isocyanates, continue to be warming up to 85～95 ℃, reaction 2～3h obtains base polyurethane prepolymer for use as, be cooled to below 50 ℃, be packaged to be the A component.
2) in the interlayer enamel reaction still, add polyether glycol by proportioning earlier, in temperature is 105～110 ℃, vacuum tightness is-and the 0.086MPa 2h that dewaters, be cooled to 60 ℃, add isocyanic ester, continue to be warming up to 75～80 ℃, reaction 3～4h adds alcohol again, reaction 2h is cooled to 50 ℃ and obtains the liquid polyurethane softening agent.
3) in the agitation vat of a 1000L, add liquid polyurethane softening agent, mixed solution, filler, pigment, auxiliary agent etc. successively, under low speed, stir 3h, grind then three times, be packaged to be the B component.
2. according to the preparation of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that the weight proportion when described A component and B component are used is: A component: B component=1: 2.
3. according to the production technique of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that polyether polyalcohol with low unsaturation degree and high molecular weight is a dibasic alcohol in the described A component, M
n=5000～12000.
4. according to the production technique of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that hydroxy silicon oil is the end capped polydimethylsiloxane of low-molecular-weight hydroxyl.Molecular formula is HO-[S
1(CH
3)
2-O]
nShown in-the H, polymerization degree n=4～11 wherein.
5. according to the production technique of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that aliphatic isocyanates is isophorone diisocyanate (IPDI), hexamethylene-diisocyanate HDI and trimer thereof etc.
6. according to the production technique of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that the polyether glycol in the liquid polyurethane softening agent is N204, N210, N220, etc. lower molecular weight two functional group's polyether glycols, isocyanic ester is isophorone diisocyanate (IPDI), hexamethylene-diisocyanate HDI and trimer thereof, TDI, MDI and modification MDI etc.Alcohol is the alcohol of single functionality, as propyl carbinol, Pentyl alcohol, n-hexyl alcohol etc.
7. according to the production technique of the polyurethane road of superior durability described in the claim 1 caulk compound, it is characterized in that mixed solution is water, surfactant mixtures.Water wherein: tensio-active agent=1: 0.1～0.2.Surface treatment agent in the mixed solution is nonionogenic tenside or anion surfactant, and water is clean tap water.
8. the filler according to polyurethane road caulking sealant with good durability described in the claim 1 is flyash, talcum powder, water-ground limestone, light calcium carbonate, nano modification water-ground limestone, aerosil, antioxidant 1010, UV-327 UV light absorber.Pigment is iron oxide red, carbon black etc.Auxiliary agent is defoamers such as fine calcium oxide.
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