CN101434825B - Bicomponent terminal mercapto polyurethane mildewproof sealant and preparation thereof - Google Patents
Bicomponent terminal mercapto polyurethane mildewproof sealant and preparation thereof Download PDFInfo
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- CN101434825B CN101434825B CN200810231465A CN200810231465A CN101434825B CN 101434825 B CN101434825 B CN 101434825B CN 200810231465 A CN200810231465 A CN 200810231465A CN 200810231465 A CN200810231465 A CN 200810231465A CN 101434825 B CN101434825 B CN 101434825B
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Abstract
The invention relates to a dual-component sulfhydryl-terminated polyurethane mildew-proof sealant and a preparation method thereof, wherein, the sealant consists of component A and component B, wherein, according to the parts by weight, the component A comprises 80-120 parts of sulfhydryl-terminated polyurethane liquid rubber, 20-200 parts of filling material, 10-100 parts of plasticizer, 0.5-10 parts of tackifier, 0.1-5 parts of mould inhibitor, 0-5 parts of vulcanization regulator, and 0-5 parts of antioxidant; the component B comprises 80-120 parts of vulcanizing agent, 20-150 parts of plasticizer, 20-200 parts of filling material, and 0-5 parts of vulcanization regulator; and the proportion of component A and component B is 10:0.5-2. The mildew-proof sealant has the tensile strength of 5.0MPa, breaking elongation rate of 1020 percent, the bonding strength with the concrete of 2.5MPa, and the mildew-proof level of being less than or equal to 1; the sealant can be used for the fields such as electrons, mechanicals, and the like, can meet the sealing and mildew-proof requirement under the conditions of long-term water immersion, damp-heat or other conditions where mildews are easy to breed, has no exhaust of three wastes and is friendly to environment.
Description
One, technical field:
The present invention relates to a kind of sealing material, particularly relate to a kind of bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof.
Two, background technology:
Seal gum is the abbreviation of sealant, is a kind of bonding and multi-usage functional materials sealing property of having simultaneously.It both can prevent internal gas or leak of liquid, can prevent intrusions such as external dust, moisture, moisture, dirt and pharmaceutical chemicals again, and can prevent mechanical vibration, impact injury or reach the effect of sound-insulating and heat-insulating.Seal gum can be out of shape with the trim shape, is difficult for trickling and certain cementability is arranged, and is widely used in the sealing of civil construction, electronic apparatus, mechanical means and communications and transportation utensil and other field component.Seal gum is indispensable important materials for solving run, drip, leak, has vital role in modern science and technology and national economy.
The main kind of seal gum has: urethane, poly-sulphur, organosilicon, acrylate, styrene-butadiene rubber(SBR), isoprene-isobutylene rubber, pitch and oiliness caulk compound etc., wherein urethane, thiorubber and organosilicon sealant performance are good, use comparatively extensively, and be called three big elastic sealants.The intensity height of polyurethane sealant, anti tear, soft wear-resisting, puncture, oil resistant and media-resistant corrosion, be widely used, isocyanate end and water in air divided reaction to discharge carbonic acid gas when shortcoming was curing, make the seal gum body produce bubble even crackle, curing speed is clamminess easily than slow and surface, moisture-proof heat and ageing-resistant adopts the then not anti-mould of natural matter synthetic urethane (semi-synthetic urethane) to corrode for a long time.
Polysulfide sealant has quite high bonding strength to concrete, metal and other base material, the resistance to air loss excellence, and the consumption allowed band of solidifying agent is wide, and solidification effect is good, the construction simple and convenient, the life-time service temperature range is-30～110 ℃.But in the process of producing thiorubber, can produce a large amount of waste water, waste residue, environment is worked the mischief.And seal gum uses in long-term hydrostatic water logging, hygrothermal environment and easily grows mould, influences sealing effectiveness.
Organosilicon sealant solidifies non-foaming, can with non-porous material surface secure bond, hydrolytic resistance, the erosion performance of anti-mould are the preferably arranged, but it is poor with the adhesiveproperties of members such as concrete, sulfuration was difficult when glue-line was thick, easily produce oily dialysis thing, pollute concrete, stone material and other jewelry, and price is more expensive.
When seal gum is used for long-term immersion of fuel tanker, boats and ships and needs or long-term hygrothermal environment, easily grow mould, along with the procreation of mould is corroded, the seal gum matrix is destroyed, influence even loss of seal effect.For guaranteeing the long term seal effect, seal gum should possess the mildew-resistant ability.Have some relevant reports both at home and abroad.Lin Yanqin etc. have reported " research of efficient mildew-resistant polysulfide sealant ", selected for use thiazoles, organometallic complex, 3 kinds of mould inhibitors of imidazoles to be applied to polysulfide sealant, prepared the good poly-sulphur mildew resistant sealant of anti-mold effect, studied the influence of mould inhibitor to sealing agent mechanical property and processing performance, find that different mould inhibitors have different influences to the mechanical property of sealing agent, and very little to the influence of processing performance.
CN200510045295.5 has invented a kind of single-component mildew-proof flame retarded organic silicon sealing agent for machinery, prepare a kind of mildew-proof flame retarded organic silicon mechanical seal glue by the method for in organic silicon sealant, adding mould inhibitor, being mainly used in the mechanical seal field. the research of at present relevant seal gum mildew-resistant focuses mostly at aircraft, boats and ships, electronics, fields such as machinery, and be used for hydro project, water delivery engineering, sewage treatment projects etc. need long-term immersion, but or long-term in hygrothermal environment, the application grow the mould mildewproof sealant product rarely seen report high easily to the sealing effectiveness requirement. if the seal gum of using in these fields does not have the antifungal function, easily grow mould, and the growth of mould and spread seal gum interior molecules structure is suffered erosion, it is rotten to produce degraded, influence even loss of seal effect.
Three, summary of the invention:
The technical problem to be solved in the present invention: a kind of polyurethane mildewproof sealant with good mechanical property and preparation method thereof is provided, sealing glue has good mechanical property, and can satisfy long-term water logging, damp and hot or other easily grow sealing and the mould proof requirement of using under the mould condition.
Technical scheme of the present invention:
A kind of bicomponent terminal mercapto polyurethane mildewproof sealant, form by A, B component, represent with weight part, wherein contain among the component A 80～120 parts of terminal mercapto polyurethane fluid rubbers, 20～200 parts of fillers, 10～100 parts in softening agent, 0.5～10 part of tackifier, 0.1～5 part of mould inhibitor; Contain 80～120 parts of vulcanizing agents, 20～150 parts in softening agent, 20～200 parts of fillers in the B component; The weight proportion of described A, B component is A: B=10: 0.5～2.
Also contain 0.5～5 part of vulcanization leveller among described component A and/or the B.
Also contain 0.5～5 part in anti-aging agent among the described component A.
Described terminal mercapto polyurethane fluid rubber is to be main chain, the end capped fluid rubber of sulfydryl with complete synthesis urethane, and 25 ℃ of viscosity are 5.0 * 10
4～40.0 * 10
4MPas, sulfydryl quality percentage composition is 1.0～2.0%, quality percentage composition≤0.2% of residual isocyano.
Described filler be lime carbonate, talcum powder, diatomite, kaolin, wollastonite, titanium dioxide, silicon-dioxide, wilkinite, zinc sulfide white and sooty any, or any two, or wantonly three kinds;
Described softening agent is any in dibutyl phthalate, dioctyl phthalate (DOP), butyl benzyl phthalate, dihexyl phthalate, diisononyl phthalate, Di Iso Decyl Phthalate, Octyl adipate, n-butyl sebacate, dioctyl sebacate, trioctyl phosphate, triphenylphosphate, Tritolyl Phosphate and the clorafin, or any two, or wantonly three kinds;
Described tackifier are octyl group phenolic tackifying resins, alkyl phenolic tackifying resin, tertiary butyl phenolic aldehyde tackifying resin, liquid-state epoxy resin, C
5In petroleum resin and the liquid coumarone indene resin any, or any two.
Described anti-aging agent is oxidation inhibitor and UV light absorber, wherein oxidation inhibitor can be antioxidant 1010 (tetramethylene (3,5-two-tertiary butyl-4-hydroxy phenylpropionic acid) methyl esters), ([3-(3 for the sulfo-di ethylene bis for oxidation inhibitor 1035,5-di-t-butyl-4 hydroxybenzene) propionic ester]), oxidation inhibitor 1024 (N, [3-(3 for N '-two, the 5-di-tert-butyl-hydroxy phenyl) propionyl] hydrazine), oxidation inhibitor 1790 (1,3,5-three-(the 4-tertiary butyl-3-hydroxyl-2, the 6-dimethyl benzyl) 1,3,5-triazine-2,4,6-(1H, 3H, 5H)-triketone), oxidation inhibitor 168 (tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester), oxidation inhibitor AT-215 (compound of antioxidant 1010 and oxidation inhibitor 168) and oxidation inhibitor PKB-215 (antioxidant 1010 or 1076 and the compound of oxidation inhibitor 168); UV light absorber can be UV light absorber UV-327 (2, the 4-tertiary butyl-6-(5-chloro benzo three imidazoles-2) phenol), UV light absorber UV-328 (2-(2H-benzotriazole base-2)-4,6-di-tert-pentyl phenol), UV light absorber UV-329 (2-(2 '-hydroxyl-5 '-the Te octyl phenyl) benzotriazole), ultraviolet absorbent UV-531 (Octabenzone) and UV light absorber Tinuvin B75 (consist of UV light absorber Tinuvin 571, hindered amine as light stabilizer Tinuvin 765 and anti-oxidant Irganox 1135 are by the mixture of the composite formation of mass ratio in 2: 2: 1); Anti-aging agent is selected from the mixture of any composition in any and the UV light absorber in the above-mentioned oxidation inhibitor.
Described mould inhibitor is any in halogenide class, heterogeneous ring compound, isothiazoline class and the quaternary ammonium salt, or any two, or wantonly three kinds; Described halogenide class is sodium pentachlorophenol, 4-chloro-2-phenylphenol or 5,6-dichloro benzoxazolone; Described heterogeneous ring compound is Top Form Wormer, benzimidazole carbamate, 1,3,5-three (2-hydroxyethyl)-s-triazine, described isothiazoline class is 1,2-benzisothiazole-3-ketone, 5-chloro-2-methyl-4-isothiazoline-3-ketone, 2-methyl-4-isothiazoline-3-ketone or 2-octyl group isothiazoline-3-ketone; Described quaternary ammonium salt is Dodecyl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, methyl tripropyl ammonium chloride, methyl tripropyl brometo de amonio, benzyl trimethyl ammonium chloride, benzyltrimethylammonium bromide, phenyl trimethyl ammonium chloride or phenyl trimethylammonium bromide.
Described vulcanizing agent is Manganse Dioxide, manganese monoxide, potassium permanganate, tellurium dioxide, antimonous oxide, zinc oxide, magnesium oxide, plumbic oxide, tri-lead tetroxide, calcium peroxide, Magnesium peroxide, hydrogen peroxide, hydrogen phosphide cumene, 2,4-tolylene diisocyanate and 2, in the 4-toluene diisocyanate dimer any, or any two, or wantonly three kinds.
Vulcanization leveller is any in stearic acid and the oleic acid in the described A component; In the described B component vulcanization leveller be in Sodium dimethyldithiocarbamate 40min, NB sodium dibutyl dithiocarbamate, ziram, zinc diethyldithiocarbamate, zinc dibutyl dithiocarbamate, tetramethylthiuram monosulfide, TBTM tetrabutyl thiuram monosulfide, tetramethyl-thiuram disulfide, tetraethylthiuram disulfide, vulkacit D, di-o-tolylguanidine and the triphenyl guanidine any, or any two, or wantonly three kinds.
A kind of preparation method of bicomponent terminal mercapto polyurethane mildewproof sealant, this method comprises the steps:
(1) preparation of antifungal sizing
Mould inhibitor in the A component and terminal mercapto polyurethane fluid rubber are joined in the kneader, under 200～1000r/min stirring velocity, stir 20～50min, stand for standby use;
(2) preparation of seal gum A component
Other material in antifungal sizing and the A component being joined in the kneader successively, stir 30～100min under 500～1200r/min stirring velocity, is 0.5 * 10 in vacuum tightness then
-4～1.0 * 10
-4Pa continues down to stir 20～50min, extrudes, and gets the A component;
(3) preparation of seal gum B component
Each material in the B component is joined in the kneader successively, under the stirring velocity of 50～200r/min, stir 10～30min, extrude, grind, get the B component.
Terminal mercapto polyurethane fluid rubber in the described A component raw material, can adopt following method preparation:
(1) (NCO) base polyurethane prepolymer for use as is synthetic: in reactor for the end isocyanato, the mixture that at first adds polyether glycol and a certain amount of an acidic catalyst, vacuum hydro-extraction 2～5 hours under 100～150 ℃ of conditions then, the add-on of an acidic catalyst is 0.1 of polyether glycol add-on～0.5 ‰, the dehydration back is the stoichiometric polyisocyanates of 1.2～2.2: 1 adding according to the mol ratio of isocyanato-NCO and hydroxyl-OH, till isothermal reaction under 60～100 ℃ of conditions is to the quality percentage composition of-NCO to theoretical value, obtain holding the isocyanato base polyurethane prepolymer for use as then;
(2) polyurethane liquid rubber is synthetic: add stoichiometric sulfhydryl compound (promptly adding the sulfhydryl compound that calculates according to chemical equation) in step (1) synthetic end isocyanato base polyurethane prepolymer for use as, under 60～120 ℃ of conditions, reaction is to quality percentage composition≤0.4% of-NCO o'clock, vacuumize, negative pressure degasification, pressure is-0.3～-0.1MPa, in reaction product till the no obvious bubble, be cooled to 40～50 ℃ after blowing.
Described polyether glycol is that molecular-weight average is that 1000～6000 polyoxypropyleneglycol, molecular-weight average are that 1000～6000 polytetrahydrofuran diol, molecular-weight average are that 1000～6000 polytetrahydrofuran-propylene oxide copolyether glycol, molecular-weight average are any dibasic alcohol in 1000～6000 polyoxytrimethylene triols and the mixture of any trivalent alcohol; Described an acidic catalyst is any in oxygen-containing inorganic acid, boric acid ester and the tartrate; Described polyisocyanates is tolylene diisocyanate TDI, 4,4 '-diphenylmethanediisocyanate MDI, PPDI PPDI, 1, any among 5-naphthalene diisocyanate NDI and the hexamethylene diisocyanate HDI; Described oxygen-containing inorganic acid is any in phosphoric acid, sulfuric acid and the nitric acid; Described boric acid ester is any in duplex isoamyl glycol borate ester, duplex (2-methyl-2,4-pentanediol) boric acid ester, duplex (2,4-dimethyl-2,4-pentanediol) boric acid ester and the duplex pyrocatechol boric acid ester; The general structure of described sulfhydryl compound is (HS)
n-R-A, wherein n is 1～3 integer, and R is any in alkane, alkene or the ether, and A is that (OH), carboxyl is (COOH) or amino (NH for hydroxyl
2) in any.
Positive beneficial effect of the present invention:
(1) to select the complete synthesis urethane that itself has strong antifungal ability for use be that main chain, the end capped fluid rubber of sulfydryl are basic glue in the present invention, composite with high-efficiency broad spectrum, low irritant, high security, low-bleed rate, compatible with bulk material, do not influence the mould inhibitor that the finished product are stored and used, adopt suitable compounded technology, prepare and have good snappiness, cementability, water tolerance, especially the seal gum that has long-term antibacterial and mouldproof ability, mildew-resistant grade≤1; Sealing glue also has excellent mechanical property, can reach 5.0MPa as tensile strength, and elongation at break reaches 1020%, can reach 2.5MPa with concrete bonding strength; In addition, working life is moderate, can satisfy the engineering construction requirement.
(2) mildewproof sealant of the present invention not only can be used for fields such as electronics, machinery, particularly can satisfy long-term water logging, damp and hot or other easily grow sealing and the mould proof requirement of using under the mould condition, but as be used for the long-term immersion of needs such as hydro project, sewage treatment project or grow the place that mould has relatively high expectations to sealing effectiveness easily at hygrothermal environment for a long time using, sealing and anti-mold effect are all better.
(3) raw material required for the present invention is easy to get, and preparation process is simple, technical maturity, and production cost is lower; And in preparation process, do not use any poisonous catalyzer and easy volatile solvent, do not have " three wastes " discharging, environmental friendliness.
Four, embodiment:
The present invention is further elaborated below in conjunction with embodiment, it should be understood that these examples only are used to illustrate concrete application note of the present invention, do not limit protection scope of the present invention.
Embodiment 1: bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof
1. bicomponent terminal mercapto polyurethane mildewproof sealant comprises A, B component
A component: terminal mercapto polyurethane fluid rubber 80kg, nano-calcium carbonate 65kg, active water-ground limestone 45kg, dibutyl phthalate 40kg, octyl group phenolic tackifying resins 1.5kg, stearic acid 1.5kg, oxidation inhibitor AT-215 1.0kg, UV light absorber UV-327 1.0kg, Top Form Wormer 1.5kg.
B component: Manganse Dioxide 80kg, dibutyl phthalate 30kg, furnace treated black 50kg, light calcium carbonate 40kg, zinc dibutyl dithiocarbamate 1.5kg.
2. the preparation method of bicomponent terminal mercapto polyurethane mildewproof sealant comprises the preparation respectively of A, B component, and concrete steps are as follows:
(1) preparation of antifungal sizing
Mould inhibitor Top Form Wormer in the A component and terminal mercapto polyurethane fluid rubber are joined in the kneader, under the 500r/min stirring velocity, stir 30min, stand for standby use;
(2) preparation of seal gum A component
Other material in antifungal sizing and the A component being joined in the kneader successively, stir 80min under the 600r/min stirring velocity, is 0.8 * 10 in vacuum tightness then
-4Pa continues down to stir 30min, extrudes, and packing gets the A component;
(3) preparation of seal gum B component
The B component is joined in the kneader successively, stir 15min under the stirring velocity of 100r/min, extrude, grind 2～5 times through three-roll grinder, packing gets the B component;
During applying glue, A, B component are with A: B=10: 1 weight ratio mixes the back and uses.
Embodiment 2: bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof
1. bicomponent terminal mercapto polyurethane mildewproof sealant comprises A, B component,
A component: terminal mercapto polyurethane fluid rubber 85kg, nano-calcium carbonate 17kg, water-ground limestone 25kg, titanium dioxide 4kg, dibutyl phthalate 30kg, octyl group phenolic tackifying resins 1.8kg, stearic acid 2.1kg, oxidation inhibitor AT-2151kg, UV light absorber UV-3281.0kg, Top Form Wormer 2.5kg.
B component: Manganse Dioxide 85kg, dibutyl phthalate 15kg, butyl benzyl phthalate 10kg, zinc dibutyl dithiocarbamate 1.5kg, light calcium carbonate 35kg.
2. the preparation method of bicomponent terminal mercapto polyurethane mildewproof sealant comprises the preparation respectively of A, B component, and concrete steps are as follows:
(1) preparation of antifungal sizing
Mould inhibitor Top Form Wormer and terminal mercapto polyurethane fluid rubber are joined in the kneader, under the 800r/min stirring velocity, stir 40min, stand for standby use;
(2) preparation of seal gum A component
Other material in antifungal sizing and the A component being joined in the kneader successively, stir 60min under the 800r/min stirring velocity, is 1.0 * 10 in vacuum tightness then
-4Pa continues down to stir 35min, extrudes, and packing gets the A component;
(3) preparation of seal gum B component
The B component is joined in the kneader successively, stir 25min under the stirring velocity of 150r/min, extrude, grind 2～5 times through three-roll grinder, packing gets the B component;
During applying glue, A, B component are with A: B=10: 0.8 weight ratio mixes the back and uses.
Embodiment 3: bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof
1. bicomponent terminal mercapto polyurethane mildewproof sealant comprises A, B component
A component: terminal mercapto polyurethane fluid rubber 90kg, nano-calcium carbonate 80kg, water-ground limestone 90kg, dibutyl phthalate 45kg, clorafin 52 45kg, octyl group phenolic tackifying resins 2.2kg, stearic acid 1.4kg, oxidation inhibitor AT-215 1.4kg, UV light absorber UV-328 1.1kg, 1,2 benzisothiazole-3-ketone 3.5kg.
B component: Manganse Dioxide 90kg, clorafin 5255kg, butyl benzyl phthalate 90kg, tetramethyl-thiuram disulfide 1.8kg, calcene 65kg.
2. the preparation method of bicomponent terminal mercapto polyurethane mildewproof sealant comprises the preparation respectively of A, B component, and concrete steps are as follows:
(1) preparation of antifungal sizing
Mould inhibitor 1,2 benzisothiazole-3-ketone and terminal mercapto polyurethane fluid rubber are joined in the kneader, under the 300r/min stirring velocity, stir 50min, stand for standby use;
(2) preparation of seal gum A component
Other material in antifungal sizing and the A component being joined in the kneader successively, stir 40min under the 1000r/min stirring velocity, is 0.9 * 10 in vacuum tightness then
-4Pa continues down to stir 45min, extrudes, and packing gets the A component;
(3) preparation of seal gum B component
Vulcanizing agent in the B component, softening agent, filler and vulcanization leveller are joined in the kneader, stir 15min under the stirring velocity of 180r/min, extrude, grind 2～5 times through three-roll grinder, packing gets the B component;
During applying glue, A, B component are with A: B=10: 1.2 weight ratio mixes the back and uses.
Embodiment 4: bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof
A component: terminal mercapto polyurethane fluid rubber 95kg, nano-calcium carbonate 48kg, wollastonite 20kg, dibutyl phthalate 50kg, alkyl phenolic tackifying resin 5kg, stearic acid 2kg, antioxidant 1010 1kg, ultraviolet absorbent UV-531 1.2kg, 5-chloro-2-methyl-4-isothiazoline-3-ketone 3kg.
B component: Manganse Dioxide 95kg, dibutyl phthalate 38kg, clorafin 52 10kg, tetramethyl-thiuram disulfide 2kg, furnace treated black 57kg, light calcium carbonate 48kg.
The preparation method of A, B component is with embodiment 1, during applying glue with A: B=10: use behind 1 the ratio mixing.
Embodiment 5: bicomponent terminal mercapto polyurethane mildewproof sealant and preparation method thereof
A component: terminal mercapto polyurethane fluid rubber 100kg, nano-calcium carbonate 90kg, water-ground limestone 55kg, wollastonite 50kg, dibutyl phthalate 50kg, clorafin 5240kg, alkyl phenolic tackifying resin 2.4kg, stearic acid 1.5kg, antioxidant 1010 1.5kg, UV light absorber UV-3281.2kg, 5,6-dichloro benzoxazolone 2kg.
B component: Manganse Dioxide 100kg, dibutyl phthalate 20kg, butyl benzyl phthalate 10kg, vulkacit D 1.2kg, furnace treated black 60kg, light calcium carbonate 30kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 0.5 the weight ratio mixing.
Embodiment 6:
A component: terminal mercapto polyurethane fluid rubber 100kg, active water-ground limestone 70kg, dibutyl phthalate 85kg, liquid-state epoxy resin 2.5kg, oleic acid 1.8kg, oxidation inhibitor AT-215 1kg, UV light absorber UV-328 1.5kg, 1,3,5-three (2-hydroxyethyl)-s-triazine 3kg.
B component: Manganse Dioxide 100kg, butyl benzyl phthalate 80kg, clorafin 52 70kg, vulkacit D 1.2kg, furnace treated black 60kg, light calcium carbonate 30kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1 the weight ratio mixing.
Embodiment 7:
A component: terminal mercapto polyurethane fluid rubber 105kg, active water-ground limestone 74kg, dibutyl phthalate 90kg, C
5Petroleum resin 3kg, oleic acid 1.9kg, antioxidant 1010 1.1kg, UV light absorber Tinuvin B75 1.6kg, 2-methyl-4 isothiazolines-3-ketone 3.2kg.
B component: Manganse Dioxide 105kg, butyl benzyl phthalate 50kg, clorafin 52 100kg, vulkacit D 2.1kg, light calcium carbonate 74kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 2 the weight ratio mixing.
Embodiment 8:
A component: terminal mercapto polyurethane fluid rubber 110kg, water-ground limestone 65kg, dibutyl phthalate 40kg, tertiary butyl phenolic aldehyde tackifying resin 2.2kg, stearic acid 2.8kg, oxidation inhibitor AT-215 1.1kg, ultraviolet absorbent UV-531 1.3kg, Top Form Wormer 2.2kg.
B component: Manganse Dioxide 110kg, clorafin 52 60kg, butyl benzyl phthalate 40kg, zinc dibutyl dithiocarbamate 3.3kg, furnace treated black 40kg, light calcium carbonate 74kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1 the weight ratio mixing.
Embodiment 9:
A component: terminal mercapto polyurethane fluid rubber 120kg, nano-calcium carbonate 80kg, water-ground limestone 120kg, dibutyl phthalate 40kg, butyl benzyl phthalate 60kg, tertiary butyl phenolic aldehyde tackifying resin 2.9kg, stearic acid 1.8kg, oxidation inhibitor AT-215 1.8kg, UV light absorber UV-329 1.5kg, benzimidazole carbamate 5kg.
B component: Manganse Dioxide 120kg, clorafin 52 90kg, butyl benzyl phthalate 60kg, zinc dibutyl dithiocarbamate 3.6kg, furnace treated black 75kg, calcene 80kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1.2 the weight ratio mixing.
Embodiment 10:
A component: terminal mercapto polyurethane fluid rubber 80kg, diatomite 20kg, dibutyl phthalate 10kg, tertiary butyl phenolic aldehyde tackifying resin 0.5kg, stearic acid 0.5kg, oxidation inhibitor 1035 1.5kg, UV light absorber UV-327 1.5kg, benzimidazole carbamate 0.1kg.
B component: Manganse Dioxide 80kg, butyl benzyl phthalate 20kg, zinc dibutyl dithiocarbamate 3.6kg, furnace treated black 5kg, calcene 5kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1.8 the weight ratio mixing.
Embodiment 11:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 10kg, oleic acid 0.5kg, oxidation inhibitor 10242kg, UV light absorber UV-329 2.5kg, benzimidazole carbamate 5kg for terminal mercapto polyurethane fluid rubber 90kg, kaolin 30kg, wilkinite 10kg, dihexyl phthalate 30kg, diisononyl phthalate 30kg, liquid-state epoxy resin.
B component: manganese monoxide 80kg, Di Iso Decyl Phthalate 40kg, Octyl adipate 20kg, Sodium dimethyldithiocarbamate 40min 2kg, titanium dioxide 75kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 2 the weight ratio mixing.
Embodiment 12:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 1kg, oleic acid 0.8kg, antioxidant 1010 2kg, UV light absorber UV-327 2.5kg, 1,2-benzisothiazole-3-ketone 4.5kg for terminal mercapto polyurethane fluid rubber 100kg, kaolin 40kg, wilkinite 10kg, n-butyl sebacate 10kg, dioctyl sebacate 30kg, liquid-state epoxy resin.
B component: potassium permanganate 20kg, manganese monoxide 80kg, Di Iso Decyl Phthalate 65kg, Octyl adipate 20kg, tetramethyl-thiuram disulfide 1kg, triphenyl guanidine 0.5kg, titanium dioxide 75kg, wollastonite 25kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 0.7 the weight ratio mixing.
Embodiment 13:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 3kg, oleic acid 5kg, oxidation inhibitor 168 0.2kg, UV light absorber UV-327 0.3kg, 1,2-octyl group isothiazoline-3-ketone 3.5kg for terminal mercapto polyurethane fluid rubber 110kg, kaolin 20kg, titanium dioxide 10kg, n-butyl sebacate 20kg, dioctyl sebacate 20kg, liquid-state epoxy resin.
B component: tellurium dioxide 20kg, antimonous oxide 80kg, n-butyl sebacate 60kg, Octyl adipate 45kg, zinc diethyldithiocarbamate 0.5kg, titanium dioxide 75kg, wollastonite 25kg, silicon-dioxide 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1 the weight ratio mixing.
Embodiment 14:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 5kg, stearic acid 0.5kg, oxidation inhibitor AT-215 1kg, UV light absorber Tinuvin B750.5kg, 1,2-benzisothiazole-3-ketone 2.5kg for terminal mercapto polyurethane fluid rubber 115kg, zinc sulfide white 30kg, carbon black 20kg, n-butyl sebacate 10kg, dioctyl sebacate 40kg, liquid-state epoxy resin.
B component: zinc oxide 40kg, magnesium oxide 80kg, Di Iso Decyl Phthalate 55kg, Octyl adipate 20kg, tetramethylthiuram monosulfide 3kg, carbon black 25kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1.2 the weight ratio mixing.
Embodiment 15:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 7kg, stearic acid 5kg, oxidation inhibitor PKB-215 0.8kg, UV light absorber UV-328 0.5kg, 2-methyl-4-isothiazoline-3-ketone 0.8kg for terminal mercapto polyurethane fluid rubber 120kg, talcum powder 30kg, wilkinite 40kg, n-butyl sebacate 30kg, clorafin 52 20kg, liquid-state epoxy resin.
B component: hydrogen peroxide 85kg, Di Iso Decyl Phthalate 60kg, clorafin 52 15kg, di-o-tolylguanidine 4kg, wollastonite 25kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1.6 the weight ratio mixing.
Embodiment 16:
The A component: (epoxy equivalent (weight) is at 170～210g/eq) 8kg, stearic acid 5kg, oxidation inhibitor 1035 0.5kg, UV light absorber UV-327 2kg, 5-chloro-2-methyl-4-isothiazoline-3-ketone 1kg for terminal mercapto polyurethane fluid rubber 85kg, silicon-dioxide 30kg, titanium dioxide 70kg, trioctyl phosphate 50kg, dioctyl sebacate 20kg, liquid-state epoxy resin.
B component: hydrogen phosphide cumene 95kg, tri-lead tetroxide 10kg, trioctyl phosphate 40kg, Octyl adipate 70kg, Sodium dimethyldithiocarbamate 40min 3kg, titanium dioxide 75kg, silicon-dioxide 80kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1.8 the weight ratio mixing.
Embodiment 17:
A component: terminal mercapto polyurethane fluid rubber 95kg, zinc sulfide white 60kg, wilkinite 30kg, n-butyl sebacate 40kg, Tritolyl Phosphate 50kg, C
5Petroleum resin 2kg, stearic acid 3kg, oxidation inhibitor 1035 1kg, UV light absorber UV-329 2kg, Dodecyl trimethyl ammonium chloride 1.5kg.
B component: 2,4 toluene diisocyanate 118kg, Di Iso Decyl Phthalate 10kg, Tritolyl Phosphate 40kg, NB sodium dibutyl dithiocarbamate 3kg, wilkinite 25kg, zinc sulfide white 10kg.
A, B method for preparing ingredients thereof be with embodiment 1, during applying glue with A: B=10: use behind 1.8 the weight ratio mixing.
Embodiment 18:
A component: terminal mercapto polyurethane fluid rubber 110kg, titanium dioxide 70kg, zinc sulfide white 50kg, Octyl adipate 30kg, dioctyl phthalate (DOP) 60kg, alkyl phenolic tackifying resin 6kg, stearic acid 1kg, oxidation inhibitor 168 2kg, UV light absorber UV-328 1.5kg, methyl tripropyl ammonium chloride 3kg.
B component: hydrogen phosphide cumene 35kg, Magnesium peroxide 60kg, Tritolyl Phosphate 40kg, clorafin 52 30kg, zinc diethyldithiocarbamate 2kg, titanium dioxide 20kg, zinc sulfide white 20kg.
A, B method for preparing ingredients thereof be with embodiment 3, during applying glue with A: B=10: use behind 0.7 the weight ratio mixing.
Embodiment 19:
The A component: terminal mercapto polyurethane fluid rubber 118kg, zinc sulfide white 140kg, n-butyl sebacate 25kg, triphenylphosphate 65kg, tertiary butyl phenolic aldehyde tackifying resin 8kg, stearic acid 1.5kg, oxidation inhibitor PKB-2151kg, UV light absorber are UV-327 3kg, benzyl trimethyl ammonium chloride 4kg.
B component: Magnesium peroxide 82kg, Octyl adipate 40kg, triphenylphosphate 30kg, vulkacit D 3kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 3, during applying glue with A: B=10: use behind 2 the weight ratio mixing.
Embodiment 20:
A component: terminal mercapto polyurethane fluid rubber 103kg, wilkinite 160kg, dibutyl phthalate 20kg, dioctyl phthalate (DOP) 40kg, butyl benzyl phthalate 50kg, tertiary butyl phenolic aldehyde tackifying resin 9.5kg, stearic acid 4.5kg, oxidation inhibitor 1790 0.8kg, UV light absorber UV-328 3kg, phenyl trimethylammonium bromide 4.5kg.
B component: 2,4 toluene diisocyanate 116kg, dibutyl phthalate 100kg, dioctyl phthalate (DOP) 18kg, butyl benzyl phthalate 10kg, tetramethyl-thiuram disulfide 4kg, wilkinite 180kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1.2 the weight ratio mixing.
Embodiment 21:
A component: terminal mercapto polyurethane fluid rubber 83kg, talcum powder 180kg, diisononyl phthalate 25kg, Di Iso Decyl Phthalate 70kg, octyl group phenolic tackifying resins 1.5kg, stearic acid 3.5kg, oxidation inhibitor 1790 2kg, UV light absorber UV-329 2kg, 2-methyl-4-isothiazoline-3-ketone 3.5kg.
B component: Manganse Dioxide 40kg, hydrogen phosphide cumene 50kg, n-butyl sebacate 40kg, dioctyl sebacate 50kg, tetraethylthiuram disulfide 1kg, wollastonite 85kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1.4 the weight ratio mixing.
Embodiment 22:
A component: terminal mercapto polyurethane fluid rubber 87kg, silicon-dioxide 200kg, triphenylphosphate 60kg, clorafin 52 40kg, alkyl phenolic tackifying resin 1kg, stearic acid 4.5kg, oxidation inhibitor AT-215 2.5kg, UV light absorber UV-513 2kg, 2-octyl group isothiazoline-3-ketone 2.5kg.
B component: 2,4 toluene diisocyanate 105kg, triphenylphosphate 80kg, clorafin 52 30kg, di-o-tolylguanidine 3kg, titanium dioxide 75kg, silicon-dioxide 80kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 0.8 the weight ratio mixing.
Embodiment 23:
A component: terminal mercapto polyurethane fluid rubber 100kg, nano-calcium carbonate 130kg, kaolin 65kg, triphenylphosphate 40kg, Tritolyl Phosphate 55kg, octyl group phenolic tackifying resins 7.5kg, stearic acid 4kg, stearic acid 2kg, oxidation inhibitor AT-215 1kg, UV light absorber Tinuvin B75 1kg, 5-chloro-2-methyl-4-isothiazoline-3-ketone 0.8kg.
B component: 2,4 toluene diisocyanate dimer 20kg, Magnesium peroxide 80kg, Di Iso Decyl Phthalate 75kg, Octyl adipate 25kg, triphenyl guanidine 0.5kg, nano-calcium carbonate 95kg, zinc sulfide white 80kg.
A, B method for preparing ingredients thereof be with embodiment 2, during applying glue with A: B=10: use behind 1.2 the weight ratio mixing.
With embodiment 1～23 prepared bicomponent terminal mercapto polyurethane mildewproof sealant, test by GB/T13477-2002 and GB/T1741-2007, the gained result is as shown in table 1:
The performance index of the bonding concrete test block of mildewproof sealant of table 1 embodiment 1-23 preparation
| Project | Working life (h) | Surface drying time (h) | Tensile strength (MPa) | Elongation at break (%) | Shore hardness (A) | Concrete bonding intensity (MPa) | The mildew-resistant grade |
| Embodiment 1 | 2.5 | 4.0 | 2.7 | 787 | 22 | 1.0 | 1 |
| Embodiment 2 | 3.0 | 4.0 | 4.8 | 650 | 37 | 2.5 | 0 |
| Embodiment 3 | 2.5 | 5.0 | 2.1 | 810 | 15 | 0.8 | 0 |
| Embodiment 4 | 1.5 | 3.0 | 3.7 | 750 | 24 | 1.3 | 0 |
| Project | Working life (h) | Surface drying time (h) | Tensile strength (MPa) | Elongation at break (%) | Shore hardness (A) | Concrete bonding intensity (MPa) | The mildew-resistant grade |
| Embodiment 5 | 4.0 | 6.0 | 1.8 | 1020 | 11 | 0.6 | 1 |
| Embodiment 6 | 1.5 | 3.0 | 1.6 | 987 | 9 | 0.4 | 0 |
| Embodiment 7 | 2.5 | 4.0 | 1.5 | 950 | 10 | 0.5 | 0 |
| Embodiment 8 | 2.0 | 3.5 | 4.6 | 670 | 35 | 2.3 | 1 |
| Embodiment 9 | 2.3 | 3.0 | 1.9 | 799 | 14 | 0.7 | 0 |
| Embodiment 10 | 1.3 | 2.0 | 5.0 | 793 | 40 | 2.4 | 1 |
| Embodiment 11 | 2.5 | 3.7 | 3.7 | 930 | 27 | 1.6 | 1 |
| Embodiment 12 | 2.0 | 3.2 | 3.9 | 680 | 32 | 2.0 | 0 |
| Embodiment 13 | 2.0 | 3.5 | 4.3 | 650 | 39 | 2.2 | 0 |
| Embodiment 14 | 1.7 | 3.0 | 4.0 | 790 | 29 | 1.9 | 1 |
| Embodiment 15 | 1.5 | 2.5 | 3.5 | 920 | 24 | 1.8 | 1 |
| Embodiment 16 | 1.3 | 3.0 | 2.1 | 850 | 20 | 1.0 | 1 |
| Embodiment 17 | 1.2 | 2.7 | 2.0 | 820 | 17 | 0.9 | 0 |
| Embodiment 18 | 2.0 | 3.1 | 2.1 | 790 | 21 | 1.1 | 1 |
| Embodiment 19 | 1.3 | 2.4 | 2.8 | 650 | 23 | 1.7 | 0 |
| Embodiment 20 | 1.5 | 2.5 | 2.3 | 870 | 20 | 1.3 | 0 |
| Embodiment 21 | 1.5 | 2.6 | 1.8 | 750 | 16 | 0.6 | 0 |
| Embodiment 22 | 2.4 | 3.2 | 1.4 | 810 | 13 | 0.5 | 0 |
| Embodiment 23 | 1.7 | 3.0 | 2.0 | 850 | 19 | 0.9 | 1 |
Claims (10)
1. bicomponent terminal mercapto polyurethane mildewproof sealant, it is characterized in that: described seal gum is made up of A, B component, represent with weight part, wherein contain 80～120 parts of terminal mercapto polyurethane fluid rubbers, 20～200 parts of fillers, 10～100 parts in softening agent, 0.5～10 part of tackifier, 0.1～5 part of mould inhibitor among the component A; Contain 80～120 parts of vulcanizing agents, 20～150 parts in softening agent, 20～200 parts of fillers in the B component; The weight ratio of described A, B component is A: B=10: 0.5～2; Described tackifier are octyl group phenolic tackifying resins, alkyl phenolic tackifying resin, tertiary butyl phenolic aldehyde tackifying resin, liquid-state epoxy resin, C
5In petroleum resin and the liquid coumarone indene resin any, or any two;
Described bicomponent terminal mercapto polyurethane mildewproof sealant preparation method comprises the steps:
(1) preparation of antifungal sizing
Mould inhibitor in the A component and terminal mercapto polyurethane fluid rubber are joined in the kneader, under 200～1000r/min stirring velocity, stir 20～50min, stand for standby use;
(2) preparation of seal gum A component
Other material in antifungal sizing and the A component being joined in the kneader successively, stir 30～100min under 500～1200r/min stirring velocity, is 0.5 * 10 in vacuum tightness then
-4～1.0 * 10
-4Pa continues down to stir 20～50min, extrudes, and gets the A component;
(3) preparation of seal gum B component
Each material in the B component is joined in the kneader successively, under the stirring velocity of 50～200r/min, stir 10～30min, extrude, grind, get the B component;
Described terminal mercapto polyurethane fluid rubber is to adopt following method preparation:
The first step: (NCO) base polyurethane prepolymer for use as is synthetic: in reactor for the end isocyanato, the mixture that at first adds polyether glycol and a certain amount of an acidic catalyst, vacuum hydro-extraction 2～5 hours under 100～150 ℃ of conditions then, the add-on of an acidic catalyst is 0.1 of polyether glycol add-on～0.5 ‰, the dehydration back is the stoichiometric polyisocyanates of 1.2～2.2: 1 adding according to the mol ratio of isocyanato-NCO and hydroxyl-OH, till isothermal reaction under 60～100 ℃ of conditions is to the quality percentage composition of-NCO to theoretical value, obtain holding the isocyanato base polyurethane prepolymer for use as then;
Second step: polyurethane liquid rubber synthetic: in step 1, add stoichiometric sulfhydryl compound in the synthetic end isocyanato base polyurethane prepolymer for use as, under 60～120 ℃ of conditions, reaction is to quality percentage composition≤0.4% of-NCO o'clock, vacuumize, negative pressure degasification, pressure is-0.3～-0.1MPa, in reaction product till the no obvious bubble, be cooled to 40～50 ℃ after blowing, promptly obtain the terminal mercapto polyurethane fluid rubber.
2. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1 is characterized in that: also contain 0.5～5 part of vulcanization leveller among described component A and the B.
3. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 2 is characterized in that; Also contain 0.5～5 part in anti-aging agent among the described component A.
4. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1 is characterized in that: described terminal mercapto polyurethane fluid rubber is to be main chain, the end capped fluid rubber of sulfydryl with complete synthesis urethane, and 25 ℃ of viscosity are 5.0 * 10
4～40.0 * 10
4MPas, sulfydryl quality percentage composition is 1.0～2.0%, quality percentage composition≤0.2% of residual isocyano.
5. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1, it is characterized in that: described filler be lime carbonate, talcum powder, diatomite, kaolin, wollastonite, titanium dioxide, silicon-dioxide, wilkinite, zinc sulfide white and sooty any, or any two, or wantonly three kinds;
Described softening agent is any in dibutyl phthalate, dioctyl phthalate (DOP), butyl benzyl phthalate, dihexyl phthalate, diisononyl phthalate, Di Iso Decyl Phthalate, Octyl adipate, n-butyl sebacate, dioctyl sebacate, trioctyl phosphate, triphenylphosphate, Tritolyl Phosphate and the clorafin, or any two, or wantonly three kinds.
6. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 3, it is characterized in that: described anti-aging agent is oxidation inhibitor and UV light absorber, and wherein oxidation inhibitor is antioxidant 1010, oxidation inhibitor 1035, oxidation inhibitor 1024, oxidation inhibitor 1790, oxidation inhibitor 168, oxidation inhibitor AT-215 and oxidation inhibitor PKB-215; UV light absorber is UV-327, UV light absorber UV-328, UV light absorber UV-329, ultraviolet absorbent UV-531 and UV light absorber Tinuvin B75; Anti-aging agent is selected from the mixture of any composition in any and the UV light absorber in the above-mentioned oxidation inhibitor.
7. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1 is characterized in that: described mould inhibitor is any in halogenide class, heterogeneous ring compound, isothiazoline class and the quaternary ammonium salt, or any two, or wantonly three kinds; Described halogenide class is sodium pentachlorophenol, 4-chloro-2-phenylphenol or 5,6-dichloro benzoxazolone; Described heterogeneous ring compound is Top Form Wormer, benzimidazole carbamate or 1,3,5-three (2-hydroxyethyl)-s-triazine; Described isothiazoline class is 1,2-benzisothiazole-3-ketone, 5-chloro-2-methyl-4-isothiazoline-3-ketone, 2-methyl-4-isothiazoline-3-ketone or 2-octyl group isothiazoline-3-ketone; Described quaternary ammonium salt is Dodecyl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, methyl tripropyl ammonium chloride, methyl tripropyl brometo de amonio, benzyl trimethyl ammonium chloride, benzyltrimethylammonium bromide, phenyl trimethyl ammonium chloride or phenyl trimethylammonium bromide.
8. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1, it is characterized in that: described vulcanizing agent is Manganse Dioxide, manganese monoxide, potassium permanganate, tellurium dioxide, antimonous oxide, zinc oxide, magnesium oxide, plumbic oxide, tri-lead tetroxide, calcium peroxide, Magnesium peroxide, hydrogen peroxide, hydrogen phosphide cumene, 2,4-tolylene diisocyanate and 2, in the 4-toluene diisocyanate dimer any, or any two, or wantonly three kinds.
9. a kind of bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 2 is characterized in that: vulcanization leveller is any in stearic acid and the oleic acid in the described A component; In the described B component vulcanization leveller be in Sodium dimethyldithiocarbamate 40min, NB sodium dibutyl dithiocarbamate, ziram, zinc diethyldithiocarbamate, zinc dibutyl dithiocarbamate, tetramethylthiuram monosulfide, TBTM tetrabutyl thiuram monosulfide, tetramethyl-thiuram disulfide, tetraethylthiuram disulfide, vulkacit D, di-o-tolylguanidine and the triphenyl guanidine any, or any two, or wantonly three kinds.
10. bicomponent terminal mercapto polyurethane mildewproof sealant according to claim 1 is characterized in that: described polyether glycol is that molecular-weight average is that 1000～6000 polyoxypropyleneglycol, molecular-weight average are that 1000～6000 polytetrahydrofuran diol, molecular-weight average are that 1000～6000 polytetrahydrofuran-propylene oxide copolyether glycol, molecular-weight average are any dibasic alcohol in 1000～6000 polyoxytrimethylene triols and the mixture of any trivalent alcohol; Described an acidic catalyst is any in oxygen-containing inorganic acid, boric acid ester and the tartrate; Described polyisocyanates is tolylene diisocyanate TDI, 4,4 '-diphenylmethanediisocyanate MDI, PPDI PPDI, 1, any among 5-naphthalene diisocyanate NDI and the hexamethylene diisocyanate HDI.
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