CN103030967B - Polyurethane grouting material - Google Patents
Polyurethane grouting material Download PDFInfo
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Abstract
The present invention relates to a kind of polyurethane grouting material, mainly in solution prior art, prepolymer method polyurethane grouting material is both needed to add solvent and plasticizer is diluted, thus the safe and environment-friendly problem in the polyurethane grouting material transport caused, construction application.The present invention is prepared by using following step: a) with isocyanate compound and polyether polyol as reaction raw materials; under inert gas shielding; under the conditions of reaction temperature is 50～90 DEG C, reaction raw materials contacts 0.5～6 hour with catalyst I, prepares grouting material performed polymer；Wherein, described catalyst I is selected from Benzenecarbonyl chloride. or phosphoric acid；B) described performed polymer is mixed homogeneously with surfactant under the conditions of 40～50 DEG C, i.e. prepare polyurethane grouting material；Wherein, described surfactant preferably solves this problem selected from the technical scheme of the water soluble silicones foam stabiliser of nonionic, can be used in the commercial production of polyurethane grouting material.
Description
Technical field
The present invention relates to a kind of polyurethane grouting material.
Background technology
Polyurethane grouting material is because of its superior performance, increasingly being widely applied in the engineerings such as water conservancy, water power, tunnel, subway, mine, people's air defense, industry and civil buildings, the particularly strengthening of foundation in engineering construction, leak stopping sealing, curtain are prevented blending the aspects such as crack repairing.
Document CN92106672.4 discloses a kind of method preparing polyurethane-type grouting material, it is to be respectively two components with isocyanate residue and hydroxy compounds, it is in the milk after Direct Uniform mixing in proportion, use after cold curing, hydroxyl compound component can use by an independent composition, can also it be that main body adds various auxiliary agent again or additive shares, these hydroxy compounds can be polyethers, polyester, polybutadiene, alkyd resin, polyacrylic resin etc..
Document CN200810052170.9 discloses the preparation method of a kind of polyurethane chemical grouting list liquid grouting chemical material, but its preparation process is divided into three steps, first hydroxyl-terminated polyurethane performed polymer is prepared, then prepare hydrophilic polyurethane performed polymer as raw material, the hydrophilic polyurethane performed polymer in the most backward step 2 adds diluent, foam stabiliser, catalyst and plasticizer and stirs and make.Long flow path, process is complicated, and containing substantial amounts of (more than 20%) low boiling point solvent acetone in product, and acetone is restricted chemicals, the usage safety performance not only making product is had a greatly reduced quality, and proposes high qualification requirement also to manufacturer's purchasing of raw materials and Product transport.
Document CN200910101168.0 discloses the soluble polyurethane chemical grouting material of a kind of high-flash (flash-point ＞ 100 DEG C) environment-friendly type.It is characterized in that being made up of isocyanates, Hydrophilicrto polyether, plasticizer and high boiling point double solvents (mixture of compound fat acid esters) and foam stabiliser.It is applicable to dam and other building Foundation Anti-seepages process, subway, Tunnel Gushing process etc..The addition of this preparation process final solvent needs to add high boiling solvent and foam stabiliser after prepolymer reaction terminates.
Therefore, in prior art, prepolymer method polyurethane grouting material is required to add the low-flash flammable solvent such as acetone, dimethylbenzene and environment, human body are poisoned big plasticizer and be diluted, and improves the flowing diffusion of slurry material with this.Owing to containing low-flash flammable liquid, general flash-point is below 61 DEG C, and therefore the fire protection requirement to job site is the highest, careless slightly major accident will be led to.Furthermore owing to these solvents, plasticizer itself have stronger volatility and toxicity, the personnel health in the underground engineerings such as subway, tunnel, culvert is constituted and greatly threatens.The most domestic high to flammable liquid transport standard-required, need special hazardous materials transportation car to transport, add the operation cost of enterprise undoubtedly, and potential danger is the biggest.
Summary of the invention
The technical problem to be solved is that in prior art, prepolymer method polyurethane grouting material is both needed to add solvent and plasticizer is diluted, thus the safe and environment-friendly problem in the polyurethane grouting material transport caused, construction application, it is provided that a kind of new polyurethane grouting material.This polyurethane grouting material, has high-flash, abnormal smells from the patient is low, toxicity is low, safety is a good feature.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows: a kind of polyurethane grouting material, is prepared by following step:
A) with isocyanate compound and polyether polyol as reaction raw materials, under inert gas shielding, under the conditions of reaction temperature is 50～90 DEG C, reaction raw materials contacts 0.5～6 hour with catalyst I, prepares grouting material performed polymer；Wherein, described catalyst I is selected from Benzenecarbonyl chloride. or phosphoric acid, and the consumption of catalyst I is the 0.05～3 ‰ of reaction raw materials weight；
B) described performed polymer is mixed homogeneously with surfactant under the conditions of 40～50 DEG C, i.e. prepare polyurethane grouting material；Wherein, described surfactant is selected from the water soluble silicones foam stabiliser of nonionic, and its consumption is the 0.3～1.0% of performed polymer weight.
In technique scheme, at least one in toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, MDI, hexamethylene-diisocyanate or poly methylene poly phenyl poly isocyanate of described isocyanate compound.Described polyether polyol is selected from two degree of functionality polyether polyol, three-functionality-degree polyether polyol and the mixture of polyether crosslinking agent；In mixture, the preferred scope of weight ratio of two degree of functionality polyether polyol, three-functionality-degree polyether polyol and polyether crosslinking agent is (16～18): (6～10): (1～3).Wherein, described two degree of functionality polyether polyol preferred versions be with propylene glycol as initiator, expoxy propane ring-opening polymerisation product, hydroxyl value is 54～120mgKOH/g；Described three-functionality-degree polyether polyol preferred version be with glycerol as initiator, expoxy propane open loop polyethers, or expoxy propane and oxirane copolyether, the preferred scope of hydroxyl value is 26～60mgKOH/g, and more preferably scope is 30～50mgKOH/g；Described polyether crosslinking agent is also a kind of three-functionality-degree polyether polyol, and the preferred scope of its hydroxyl value is 150～600mgKOH/g.Described surfactant preferred version is selected from water soluble silicones surfactant.The preferred scope of step a) reaction temperature is 75～85 DEG C, and response time preferred scope is 2～4 hours, the preferred scope of consumption is reaction raw materials weight the 0.1～2 ‰ of catalyst.The preferred scope of consumption is performed polymer weight the 0.4～0.7% of step b) surfactant.Step b) preferred version is described performed polymer when mixing with surfactant, for making the grouting material foamed solidification time can regulate in wider range, is additionally added catalyst II；Wherein, catalyst II is selected from double dimethylaminoethyl ether, N, at least one in N-dimethyl cyclohexyl amine, N-ethylmorpholine, N-methylmorpholine, N,N-Dibenzylamine or N-cocoa morpholine, preferred version is at least one in double dimethylaminoethyl ethers, N,N-Dibenzylamine or N-cocoa morpholine；The consumption of catalyst II be the 2～8% of performed polymer weight, preferably scope be the 3～6% of performed polymer weight.In described performed polymer, the preferred scope of the weight percentage of NCO is 15～28%, and more preferably scope is ＞ 22～28%.
The polyurethane grouting material of the present invention, uses raw material little to environment and physical effects, that toxicity is low in preparation process, and without any organic solvent and any plasticizer in product, the concrete castability simultaneously having taken into account product meets downstream construction application requirement.The grouting material of the present invention, frothing percentage is high, and setting time is short, the waterproofing and leakage-stopping function admirable of product；Particularly because product is the component of polymer of 100%, without organic solvent (high volatilization, low-flash, low boiling, toxicity) and plasticizer (to bad environmental), the flash-point of material is up to 162 DEG C, security performance and the environmental-protecting performance of product are greatly enhanced, can effectively stop the serious accidents such as the combustion explosion that flammable solvent type product in use produces, advantageous particularly to underground confined space construction application；Meanwhile, viscosity is less than 1000mpa.s (25 DEG C), and by the selection of polyethers with control performed polymer NCO content, the viscosity of product can as little as 500mpa.s, it is possible to meets construction application requirement, achieves preferable technique effect.
In performed polymer of the present invention the content of NCO can pass through HGT2409-1992 (mensuration of isocyanate group content in base polyurethane prepolymer for use as) analyze determine.
Surfactant used in the present invention is selected from the water soluble silicones foam stabiliser of nonionic, preferred version is selected from water soluble silicones surfactant, such as: DabcoDC190, DabcoDC5900, DabcoDC5604, DabcoDC5555, NiaxL-580, NiaxL-620, NiaxL-632, NiaxL-5770.
The polyurethane grouting material of the present invention, the evaluation methodology of its performance is as follows: weigh polyurethane grouting material 40 grams, adds catalyst 2, after mix homogeneously, adds 2 grams of water, stir rapidly, and serosity starts foaming, and height rises, and volume increases until foaming stops.Test frothing percentage and setting time.
The mensuration of frothing percentage: after polyurethane grouting material reacts with water, the cystose induration of formation, relative to the volume rate of increase of virgin pulp liquid, is expressed as a percentage.Calculate as follows:
In formula: Fc is frothing percentage；V1 is the volume before polyurethane grouting material consolidation；V2 is the volume of foam after foaming.
The mensuration of setting time: after polyurethane grouting material mixes with catalyst, water, foaming body stops being considered as setting time when rising.
Below by embodiment, the invention will be further elaborated.
Detailed description of the invention
[embodiment 1]
10 grams of polyether crosslinking agent, 65 grams of polyether polyol B, 30 grams of polyether polyol C, 0.7 gram of Benzenecarbonyl chloride. are put in 1000 milliliters of there-necked flasks; analysis moisture; moisture should≤0.05% (if defective; intensification vacuum dehydration is until qualified); put into 200 grams of poly methylene poly phenyl poly isocyanates and 105 grams of MDIs; nitrogen charging gas shield; stirring heats up; constant temperature keeps 1 hour at 55 DEG C; then proceed to be warming up to 78 DEG C; keep 3 hours, prepare grouting resin prepolymer.
The grouting resin prepolymer of preparation dimethylaminoethyl ethers double with organic silicon surfactant DabcoDC190, catalyst II under the conditions of 42 DEG C are mixed homogeneously, obtains polyurethane grouting material.
Wherein, polyether crosslinking agent hydroxyl value is 500mgKOH/g；Polyether polyol B bis-degree of functionality polyether polyol hydroxyl value is 112mgKOH/g；Polyether polyol C three-functionality-degree polyether polyol hydroxyl value is 56mgKOH/g.Performed polymer is 100: 0.6 with the weight ratio of surfactant, consumption is performed polymer weight the 2% of double dimethylaminoethyl ethers.In performed polymer, the content of NCO is 21.1%.
The polyurethane grouting material prepared is light brown viscous liquid, has no irritating odor, and technical specification is shown in Table 1.
[embodiment 2].
9 grams of polyether crosslinking agent, 83 grams of polyether polyol B, 42 grams of polyether polyol C, 0.14 gram of phosphoric acid solution are put in 1000 milliliters of there-necked flasks; analysis moisture; moisture should≤0.05% (if defective; intensification vacuum dehydration is until qualified); put into 276 grams of poly methylene poly phenyl poly isocyanates and 184 grams of MDIs; nitrogen charging gas shield; heat up after stirring 30 minutes; constant temperature keeps 1 hour at 55 DEG C; then proceed to be warming up to 82 DEG C; keep 3 hours, prepare grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed homogeneously with surfactant D abcoDC5900, catalyst IIN-ethyl morpholine under the conditions of 45 DEG C, obtains polyurethane grouting material.
Wherein, polyether crosslinking agent hydroxyl value is 500mgKOH/g；Polyether polyol B bis-degree of functionality polyether polyol hydroxyl value is 56mgKOH/g；Polyether polyol C three-functionality-degree polyether polyol hydroxyl value is 48mgKOH/g.Performed polymer is 100: 0.42 with the weight ratio of surfactant, and the consumption of catalyst II is the 6% of performed polymer weight.In performed polymer, the content of NCO is 22.6%.
The polyurethane grouting material prepared is light brown viscous liquid, has no irritating odor, and technical specification is shown in Table 1.
[embodiment 3].
250 grams of polyether crosslinking agent, 2100 grams of polyether polyol B, 1000 grams of polyether polyol C, 15 grams of phosphoric acid solutions are put in 20 liters of pressure reactors of rustless steel; analysis moisture; moisture should≤0.05% (if defective; intensification vacuum dehydration is until qualified); put into 5530 grams of poly methylene poly phenyl poly isocyanates and 5990 grams of MDIs; nitrogen charging gas shield; heat up after stirring 30 minutes; constant temperature keeps 1 hour at 60 DEG C; then proceed to be warming up to 85 DEG C; keep 2.0 hours, prepare grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed homogeneously with surfactant NiaxL-632, catalyst II N,N-Dibenzylamine under the conditions of 45 DEG C, obtains polyurethane grouting material.
Wherein, polyether crosslinking agent hydroxyl value is 330mgKOH/g；Polyether polyol B bis-degree of functionality polyether polyol hydroxyl value is 56mgKOH/g；Polyether polyol C three-functionality-degree polyether polyol hydroxyl value is 56mgKOH/g.Performed polymer is 100: 0.54 with the weight ratio of surfactant, and the consumption of catalyst II is the 5% of performed polymer weight.In performed polymer, the content of NCO is 23.5%.
The polyurethane grouting material prepared is light brown viscous liquid, has no irritating odor, and technical specification is shown in Table 1.
[embodiment 4]
315 grams of polyether crosslinking agent, 2550 grams of polyether polyol B, 1275 grams of polyether polyol C, 30 grams of phosphoric acid are put in reactor; analysis moisture; moisture should≤0.05% (if defective; intensification vacuum dehydration is until qualified); put into 5540 grams of poly methylene poly phenyl poly isocyanates and 6000 grams of MDIs; nitrogen charging gas shield; heat up after stirring 30 minutes; constant temperature keeps 1 hour at 60 DEG C; then proceed to be warming up to 85 DEG C; keep 2.5 hours, prepare grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed homogeneously with surfactant NiaxL-580, catalyst IIN-methyl morpholine under the conditions of 50 DEG C, obtains polyurethane grouting material.
Wherein, polyether crosslinking agent hydroxyl value is 330mgKOH/g；Polyether polyol B bis-degree of functionality polyether polyol hydroxyl value is 56mgKOH/g；Polyether polyol C three-functionality-degree polyether polyol hydroxyl value is 35mgKOH/g.Performed polymer is 100: 0.51 with the weight ratio of surfactant, and the consumption of catalyst II is the 7% of performed polymer weight.In performed polymer, the content of NCO is 22.4%.
The polyurethane grouting material prepared is light brown viscous liquid, has no irritating odor, and technical specification is shown in Table 1.
[embodiment 5]
56 kilograms of polyether crosslinking agent, 450 kilograms of polyether polyol B, 225 kilograms of grams of polyether polyol C, 3 kilograms of Benzenecarbonyl chloride .s are put into 5 meters3In stainless steel cauldron; analysis moisture; moisture should≤0.05% (if defective, intensification vacuum dehydration is until qualified), put into 1148 kilograms of poly methylene poly phenyl poly isocyanates and 1102 kilograms of MDIs; nitrogen charging gas 1 kilogram protection; heating up after stirring 30 minutes, constant temperature keeps 1 at 60 DEG C, then proceedes to be warming up to 82 DEG C; keep 2.5 hours, prepare grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed homogeneously with surfactant D abcoDC5555, catalyst IIN-cocoa morpholine under the conditions of 50 DEG C, obtains polyurethane grouting material.
Wherein, polyether crosslinking agent hydroxyl value is 170mgKOH/g；Polyether polyol B bis-degree of functionality polyether polyol hydroxyl value is 56mgKOH/g；Polyether polyol C three-functionality-degree polyether polyol hydroxyl value is 35mgKOH/g.Performed polymer is 100: 0.9 with the weight ratio of surfactant, and the consumption of catalyst II is the 4.5% of performed polymer weight.In performed polymer, the content of NCO is 23%.
The polyurethane grouting material prepared is light brown viscous liquid, has no irritating odor, and technical specification is shown in Table 1.
[comparative example]
Grouting material is prepared according to method disclosed in document CN200810052170.9.The grouting material prepared has strong impulse abnormal smells from the patient.Technical specification is shown in Table 1.
Table 1
Claims (8)
1. a polyurethane grouting material, is prepared by following step:
A) with isocyanate compound and polyether polyol as reaction raw materials, under inert gas shielding, under the conditions of reaction temperature is 50～90 DEG C, reaction raw materials contacts 0.5～6 hour with catalyst I, prepares grouting material performed polymer；Wherein, described catalyst I is selected from Benzenecarbonyl chloride. or phosphoric acid, and the consumption of catalyst I is the 0.05～3 ‰ of reaction raw materials weight；
B) described performed polymer is mixed homogeneously with surfactant under the conditions of 40～50 DEG C, i.e. prepare polyurethane grouting material；Wherein, described surfactant is selected from the water soluble silicones foam stabiliser of nonionic, and its consumption is the 0.3～1.0% of performed polymer weight；
Described polyether polyol is selected from two degree of functionality polyether polyol, three-functionality-degree polyether polyol and the mixture of polyether crosslinking agent；In mixture, the weight ratio of two degree of functionality polyether polyol, three-functionality-degree polyether polyol and polyether crosslinking agent is (16～18): (6～10): (1～3)；
Described polyurethane grouting material is the component of polymer of 100%, without organic solvent and plasticizer.
Polyurethane grouting material the most according to claim 1, it is characterised in that at least one in toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, hexamethylene-diisocyanate or poly methylene poly phenyl poly isocyanate of described isocyanate compound.
Polyurethane grouting material the most according to claim 1, it is characterised in that described two degree of functionality polyether polyol be with propylene glycol as initiator, expoxy propane ring-opening polymerisation product, hydroxyl value is 54～120mgKOH/g；Described three-functionality-degree polyether polyol be with glycerol as initiator, expoxy propane open loop polyethers, or expoxy propane and oxirane copolyether, hydroxyl value is 28～56mgKOH/g；Described polyether crosslinking agent hydroxyl value is 150～600mgKOH/g.
Polyurethane grouting material the most according to claim 1, it is characterised in that when the described performed polymer of step b) mixes with surfactant, be additionally added catalyst II；Wherein, catalyst II is selected from double dimethylaminoethyl ether, N, and at least one in N-dimethyl cyclohexyl amine, N-ethylmorpholine, N-methylmorpholine, N,N-Dibenzylamine or N-cocoa morpholine, its consumption is the 2～8% of performed polymer weight.
Polyurethane grouting material the most according to claim 4, it is characterised in that at least one in double dimethylaminoethyl ethers, N,N-Dibenzylamine or N-cocoa morpholine of described catalyst II, its consumption is the 3～6% of performed polymer weight.
Polyurethane grouting material the most according to claim 1, it is characterised in that step a) reaction temperature is 75～85 DEG C, the response time is 2～4 hours, and the consumption of catalyst is the 0.1～2 ‰ of reaction raw materials weight；Consumption is performed polymer weight the 0.4～0.7% of step b) surfactant.
Polyurethane grouting material the most according to claim 1, it is characterised in that in described performed polymer, the weight percentage of NCO is 15～28%.
Polyurethane grouting material the most according to claim 7, it is characterised in that in described performed polymer, the weight percentage of NCO is > 22～28%.
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| 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 |
| CN108047699A (en) * | 2017-12-13 | 2018-05-18 | 上海东大化学有限公司 | A kind of environment-friendly type large arch dam hydrophobic polyurethane grout composition and preparation method thereof |
| CN110511352A (en) * | 2019-09-09 | 2019-11-29 | 中交（广州）建设有限公司 | Water blockoff polyurethane injecting paste material and preparation method thereof is reinforced in a kind of filling |
| CN110684166B (en) * | 2019-09-25 | 2021-11-30 | 佛山市日凯科技有限公司 | Foaming grouting agent |
| CN115960589B (en) * | 2021-10-11 | 2024-02-20 | 中国石油化工股份有限公司 | Composition for preparing grouting material for well drilling plugging |
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