CN103030967A - Polyurethane grouting material - Google Patents
Polyurethane grouting material Download PDFInfo
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- CN103030967A CN103030967A CN201110303153XA CN201110303153A CN103030967A CN 103030967 A CN103030967 A CN 103030967A CN 201110303153X A CN201110303153X A CN 201110303153XA CN 201110303153 A CN201110303153 A CN 201110303153A CN 103030967 A CN103030967 A CN 103030967A
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- polyurethane grouting
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Abstract
The invention relates to a polyurethane grouting material, mainly aiming at solving safety and environmental problems during transportation and construction application of the polyurethane grouting material caused by that the existing polyurethane grouting material obtained through a prepolymerization method in the prior art is required to be diluted by adding solvent and plasticizer. The polyurethane grouting material is prepared through a method which comprises the following steps of: a) taking isocyanate compounds and polyether polyol as reaction raw materials, and enabling the reaction raw materials to be in contact with catalyst I for 0.5-6 hours at reaction temperature of 50-90DEG C under the protection of inert gas to obtain grouting material prepolymers, wherein the catalyst I is benzoyl chloride or phosphoric acid; and b) evenly mixing the prepolymers with surfactant at 40-50DEG C to obtain the polyurethane grouting material, wherein the surfactant is nonionic water-soluble polysiloxane foam. By adopting the technical scheme, the problems are better solved and the method is suitable for the industrial production of the 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, obtain using more and more widely in the engineerings such as water conservancy, water power, tunnel, subway, mine, people's air defense, industry and covil construction, the particularly strengthening of foundation in engineering construction, leak stopping sealing, curtain prevent blending the aspects such as crack repairing.
Document CN92106672.4 discloses a kind of method for preparing the polyurethane-type injection material, to be respectively two components with isocyanate residue and oxy-compound, Direct Uniform is in the milk after mixing in proportion, use after the self-vulcanizing, the oxy-compound component can be used by an independent composition, can it be that main body is added various auxiliary agents again or additive shares also, these oxy-compound can be polyethers, polyester, polyhutadiene, Synolac, polyacrylic resin etc.
Document CN200810052170.9 discloses a kind of preparation method of polyurethane chemical grouting list liquid grouting chemical material, but its preparation process is divided into three steps, at first prepare the hydroxyl-terminated polyurethane performed polymer, then prepare the hydrophilic polyurethane performed polymer as raw material, add thinner, suds-stabilizing agent, catalyzer and softening agent in the hydrophilic polyurethane performed polymer in the most backward step 2 and stir and make.Long flow path, process is complicated, and contains a large amount of (more than 20%) low boiling point solvent acetone in the product, and acetone is restricted chemical, the usage safety performance of product is had a greatly reduced quality, proposed high qualification requirement also for 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 point (flash-point＞100 ℃) environment-friendly type.It is characterized in that being formed by isocyanic ester, Hydrophilicrto polyether, softening agent and high boiling point double solvents (mixture of compound fat acid esters) and suds-stabilizing agent.Be applicable to dam and other building foundation antiseepage processing, subway, Tunnel Gushing processing etc.The adding of this preparation process final solvent need to add high boiling solvent and suds-stabilizing agent after prepolymer reaction finishes.
Therefore the prepolymer method polyurethane grouting material all needs to add the low-flash flammable solvent such as acetone, dimethylbenzene and environment, human body is poisoned large softening agent dilute in the prior art, improves the flow expansion performance of slurry material with this.Owing to contain the low-flash inflammable liquid, general flash-point all is lower than 61 ℃, and is therefore very high to the fire protection requirement of working-yard, careless slightlyly will lead to Serious Accident.Moreover owing to these solvents, softening agent itself have stronger volatility and toxicity, consist of greatly threat for the personnel health in the underground workss such as subway, tunnel, culvert.Simultaneously domestic high to inflammable liquid transportation standard-required, need special carriage of dangerous goods car transportation, increased undoubtedly the operation cost of enterprise, and potential danger is also large.
Summary of the invention
Technical problem to be solved by this invention is that the prepolymer method polyurethane grouting material all need add solvent and softening agent dilutes in the prior art, thereby safety, environmental issue in the polyurethane grouting material that causes transportation, the construction application provide a kind of new polyurethane grouting material.This polyurethane grouting material has high flash point, smell is low, toxicity is low, security is good characteristics.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of polyurethane grouting material prepares by following step:
A) take isocyanate compound and polyether glycol as reaction raw materials, under protection of inert gas, be under 50～90 ℃ of conditions in temperature of reaction, reaction raw materials contacts 0.5～6 hour with catalyst I, make the injection material performed polymer; Wherein, described catalyst I is selected from Benzoyl chloride or phosphoric acid, and the consumption of catalyst I is 0.05 of reaction raw materials weight～3 ‰;
B) described performed polymer and tensio-active agent are mixed under 40～50 ℃ of conditions, namely make polyurethane grouting material; Wherein, described tensio-active agent is selected from the water-soluble poly siloxane foams stablizer of non-ionic type, and its consumption is 0.3～1.0% of performed polymer weight.
In the technique scheme, described isocyanate compound is selected from least a in tolylene diisocyanate, diphenylmethanediisocyanate, MDI, hexamethylene-diisocyanate or the poly methylene poly phenyl poly isocyanate.Described polyether glycol is selected from the mixture of two functionality polyether glycols, three-functionality-degree polyether glycol and polyether crosslinking agent; In the mixture, the weight ratio preferable range of two functionality polyether glycols, three-functionality-degree polyether glycol and polyether crosslinking agent is (16～18): (6～10): (1～3).Wherein, described two functionality polyether glycol preferred versions for take propylene glycol as initiator, propylene oxide ring-opening polymerization product, hydroxyl value is 54～120mgKOH/g; Described three-functionality-degree polyether glycol preferred version for take glycerine as initiator, propylene oxide open loop polyethers, perhaps propylene oxide and oxyethane copolyether, the hydroxyl value preferable range is 26～60mgKOH/g, more preferably scope is 30～50mgKOH/g; Described polyether crosslinking agent also is a kind of three-functionality-degree polyether glycol, and its hydroxyl value preferable range is 150～600mgKOH/g.Described tensio-active agent preferred version is for being selected from the water-soluble poly silicone surfactant.Step a) temperature of reaction preferable range is 75～85 ℃, and the reaction times preferable range is 2～4 hours, and the consumption preferable range of catalyzer is 0.1 of reaction raw materials weight～2 ‰.Step b) the consumption preferable range of tensio-active agent is 0.4～0.7% of performed polymer weight.Step b) preferred version is described performed polymer when mixing with tensio-active agent, can more regulate in the wide region for making the injection material foamed solidification time, also adds catalyst I I; Wherein, catalyst I I is selected from two dimethylaminoethyl ethers, N, at least a in N-dimethylcyclohexylamine, N-ethylmorpholine, N-methylmorpholine, N,N-Dibenzylamine or the N-cocoa morpholine, preferred version are to be selected from least a in two dimethylaminoethyl ethers, N,N-Dibenzylamine or the N-cocoa morpholine; The consumption of catalyst I I is 2～8% of performed polymer weight, and preferable range is 3～6% of performed polymer weight.The weight percentage preferable range of NCO is 15～28% in the described performed polymer, and more preferably scope is＞22～28%.
Polyurethane grouting material of the present invention adopts the raw material little to environment and physical effects, that toxicity is low in preparation process, do not add any organic solvent and any softening agent in the product, and the concrete castability of having taken into account simultaneously product satisfies downstream construction application requirement.Injection material of the present invention, frothing percentage is high, and setting time is short, the waterproofing and leakage-stopping excellent property of product; It is special because product is 100% component of polymer, do not contain organic solvent (high volatilization, low-flash, lower boiling, toxicity) and softening agent (harmful to environment), the flash-point of material is up to 162 ℃, safety performance and the environmental-protecting performance of product are greatly enhanced, can effectively stop the serious accidents such as combustion explosion that flammable solvent type product in use produces, advantageous particularly to underground enclosed space construction application; Simultaneously, viscosity is lower than 1000mpa.s (25 ℃), and by selection and the control performed polymer NCO content of polyethers, the viscosity of product can be low to moderate 500mpa.s, can satisfy the construction application requirement, has obtained preferably technique effect.
The content of NCO can pass through HGT2409-1992 (mensuration of isocyanate group content in the base polyurethane prepolymer for use as) Analysis deterrmination in the performed polymer of the present invention.
Used tensio-active agent is selected from the water-soluble poly siloxane foams stablizer of non-ionic type among the present invention, preferred version is for being selected from the water-soluble poly silicone surfactant, for example: Dabco DC190, Dabco DC5900, Dabco DC5604, Dabco DC5555, Niax L-580, Niax L-620, Niax L-632, Niax L-5770.
Polyurethane grouting material of the present invention, the evaluation method of its performance is as follows: take by weighing polyurethane grouting material 40 grams, add catalyzer 2, after mixing, add 2 gram water again, stir rapidly, slurries begin foaming, highly rise, and volume increases until foaming stops.Test frothing percentage and setting time.
The mensuration of frothing percentage: after polyurethane grouting material and the water reaction, the spumescence induration of formation represents with per-cent with respect to the volume growth rate of virgin pulp liquid.Calculate as follows:
In the formula: Fc is frothing percentage; V 1 is the fixed front volume of polyurethane grouting material; V 2 is the volume of the rear foam of foaming.
The mensuration of setting time: polyurethane grouting material is considered as setting time with after catalyzer, water mix when foam stops to rise.
The invention will be further elaborated below by embodiment.
Embodiment
[embodiment 1]
10 gram polyether crosslinking agent, 65 gram polyether glycol B, 30 gram polyether glycol C, 0.7 gram Benzoyl chloride are dropped in 1000 milliliters of there-necked flasks; analysis moisture; moisture content is should≤0.05% (if defective; intensification vacuum hydro-extraction is until qualified); drop into 200 gram poly methylene poly phenyl poly isocyanates and 105 gram MDIs; the protection of inflated with nitrogen body; stir and heat up; constant temperature kept 1 hour at 55 ℃; then continue to be warming up to 78 ℃; kept 3 hours, and made the grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed with the two dimethylaminoethyl ethers of organic silicon surfactant Dabco DC190, catalyst I I under 42 ℃ of conditions, obtain polyurethane grouting material.
Wherein, the polyether crosslinking agent hydroxyl value is 500mgKOH/g; Polyether glycol B two functionality polyether glycol hydroxyl values are 112mgKOH/g; Polyether glycol C three-functionality-degree polyether glycol hydroxyl value is 56mgKOH/g.The weight ratio of performed polymer and tensio-active agent is 100: 0.6, and the consumption of two dimethylaminoethyl ethers is 2% of performed polymer weight.The content of NCO is 21.1% in the performed polymer.
The urethane grouting material that makes is light brown viscous liquid, has no irritating odor, and technical indicator sees Table 1.
[embodiment 2].
9 gram polyether crosslinking agent, 83 gram polyether glycol B, 42 gram polyether glycol C, 0.14 gram phosphoric acid solution are dropped in 1000 milliliters of there-necked flasks; analysis moisture; moisture content is should≤0.05% (if defective; intensification vacuum hydro-extraction is until qualified); drop into 276 gram poly methylene poly phenyl poly isocyanates and 184 gram MDIs; the protection of inflated with nitrogen body; stir after 30 minutes and heat up; constant temperature kept 1 hour at 55 ℃; then continue to be warming up to 82 ℃; kept 3 hours, and made the grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed with surfactant D abco DC5900, catalyst I IN-ethyl morpholine under 45 ℃ of conditions, obtain polyurethane grouting material.
Wherein, the polyether crosslinking agent hydroxyl value is 500mgKOH/g; Polyether glycol B two functionality polyether glycol hydroxyl values are 56mgKOH/g; Polyether glycol C three-functionality-degree polyether glycol hydroxyl value is 48mgKOH/g.The weight ratio of performed polymer and tensio-active agent is 100: 0.42, and the consumption of catalyst I I is 6% of performed polymer weight.The content of NCO is 22.6% in the performed polymer.
The urethane grouting material that makes is light brown viscous liquid, has no irritating odor, and technical indicator sees Table 1.
[embodiment 3].
250 gram polyether crosslinking agent, 2100 gram polyether glycol B, 1000 gram polyether glycol C, 15 gram phosphoric acid solutions are dropped in 20 liters of withstand voltage reactors of stainless steel; analysis moisture; moisture content is should≤0.05% (if defective; intensification vacuum hydro-extraction is until qualified); drop into 5530 gram poly methylene poly phenyl poly isocyanates and 5990 gram MDIs; the protection of inflated with nitrogen body; stir after 30 minutes and heat up; constant temperature kept 1 hour at 60 ℃; then continue to be warming up to 85 ℃; kept 2.0 hours, and made the grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed with tensio-active agent Niax L-632, catalyst I I N,N-Dibenzylamine under 45 ℃ of conditions, obtain polyurethane grouting material.
Wherein, the polyether crosslinking agent hydroxyl value is 330mgKOH/g; Polyether glycol B two functionality polyether glycol hydroxyl values are 56mgKOH/g; Polyether glycol C three-functionality-degree polyether glycol hydroxyl value is 56mgKOH/g.The weight ratio of performed polymer and tensio-active agent is 100: 0.54, and the consumption of catalyst I I is 5% of performed polymer weight.The content of NCO is 23.5% in the performed polymer.
The urethane grouting material that makes is light brown viscous liquid, has no irritating odor, and technical indicator sees Table 1.
[embodiment 4]
315 gram polyether crosslinking agent, 2550 gram polyether glycol B, 1275 gram polyether glycol C, 30 gram phosphoric acid are dropped in the reactor; analysis moisture; moisture content is should≤0.05% (if defective; intensification vacuum hydro-extraction is until qualified); drop into 5540 gram poly methylene poly phenyl poly isocyanates and 6000 gram MDIs; the protection of inflated with nitrogen body; stir after 30 minutes and heat up; constant temperature kept 1 hour at 60 ℃; then continue to be warming up to 85 ℃; kept 2.5 hours, and made the grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed with tensio-active agent Niax L-580, catalyst I IN-methylmorpholine under 50 ℃ of conditions, obtain polyurethane grouting material.
Wherein, the polyether crosslinking agent hydroxyl value is 330mgKOH/g; Polyether glycol B two functionality polyether glycol hydroxyl values are 56mgKOH/g; Polyether glycol C three-functionality-degree polyether glycol hydroxyl value is 35mgKOH/g.The weight ratio of performed polymer and tensio-active agent is 100: 0.51, and the consumption of catalyst I I is 7% of performed polymer weight.The content of NCO is 22.4% in the performed polymer.
The urethane grouting material that makes is light brown viscous liquid, has no irritating odor, and technical indicator sees Table 1.
[embodiment 5]
56 kilograms of polyether crosslinking agent, 450 kilograms of polyether glycol B, 225 kilograms of gram polyether glycol C, 3 kilograms of Benzoyl chlorides are dropped into 5 meters
3In the stainless steel cauldron; analysis moisture; moisture content is answered≤0.05% (if defective, intensification vacuum hydro-extraction is until qualified), drops into 1148 kilograms of poly methylene poly phenyl poly isocyanates and 1102 kilograms of MDIs; 1 kilogram of protection of inflated with nitrogen body; stir after 30 minutes and heat up, constant temperature keeps 1 at 60 ℃, then continues to be warming up to 82 ℃; kept 2.5 hours, and made the grouting resin prepolymer.
The grouting resin prepolymer of preparation is mixed with surfactant D abco DC5555, catalyst I IN-cocoa morpholine under 50 ℃ of conditions, obtain polyurethane grouting material.
Wherein, the polyether crosslinking agent hydroxyl value is 170mgKOH/g; Polyether glycol B two functionality polyether glycol hydroxyl values are 56mgKOH/g; Polyether glycol C three-functionality-degree polyether glycol hydroxyl value is 35mgKOH/g.The weight ratio of performed polymer and tensio-active agent is 100: 0.9, and the consumption of catalyst I I is 4.5% of performed polymer weight.The content of NCO is 23% in the performed polymer.
The urethane grouting material that makes is light brown viscous liquid, has no irritating odor, and technical indicator sees Table 1.
[comparative example]
Prepare injection material according to the disclosed method of document CN200810052170.9.The injection material that makes has the strong impulse smell.Technical indicator sees Table 1.
Table 1
Claims (10)
1. polyurethane grouting material, by following step preparation:
A) take isocyanate compound and polyether glycol as reaction raw materials, under protection of inert gas, be under 50～90 ℃ of conditions in temperature of reaction, reaction raw materials contacts 0.5～6 hour with catalyst I, make the injection material performed polymer; Wherein, described catalyst I is selected from Benzoyl chloride or phosphoric acid, and the consumption of catalyst I is 0.05 of reaction raw materials weight～3 ‰;
B) described performed polymer and tensio-active agent are mixed under 40～50 ℃ of conditions, namely make polyurethane grouting material; Wherein, described tensio-active agent is selected from the water-soluble poly siloxane foams stablizer of non-ionic type, and its consumption is 0.3～1.0% of performed polymer weight.
2. polyurethane grouting material according to claim 1 is characterized in that described isocyanate compound is selected from least a in tolylene diisocyanate, diphenylmethanediisocyanate, MDI, hexamethylene-diisocyanate or the poly methylene poly phenyl poly isocyanate.
3. polyurethane grouting material according to claim 1 is characterized in that described polyether glycol is selected from the mixture of two functionality polyether glycols, three-functionality-degree polyether glycol and polyether crosslinking agent; In the mixture, the weight ratio of two functionality polyether glycols, three-functionality-degree polyether glycol and polyether crosslinking agent is (16～18): (6～10): (1～3).
4. polyurethane grouting material according to claim 3, it is characterized in that described two functionality polyether glycols for take propylene glycol as initiator, propylene oxide ring-opening polymerization product, hydroxyl value is 54～120mgKOH/g; Described three-functionality-degree polyether glycol for take glycerine as initiator, propylene oxide open loop polyethers, perhaps propylene oxide and oxyethane copolyether, hydroxyl value is 28～56mgKOH/g; Described polyether crosslinking agent hydroxyl value is 150～600mgKOH/g.
5. polyurethane grouting material according to claim 1 is characterized in that described tensio-active agent is selected from the water-soluble poly silicone surfactant.
6. polyurethane grouting material according to claim 1 is characterized in that step b) when described performed polymer mixes with tensio-active agent, also add catalyst I I; Wherein, catalyst I I is selected from two dimethylaminoethyl ethers, N, at least a in N-dimethylcyclohexylamine, N-ethylmorpholine, N-methylmorpholine, N,N-Dibenzylamine or the N-cocoa morpholine, and its consumption is 2～8% of performed polymer weight.
7. polyurethane grouting material according to claim 6 is characterized in that described catalyst I I is selected from least a in two dimethylaminoethyl ethers, N,N-Dibenzylamine or the N-cocoa morpholine, and its consumption is 3～6% of performed polymer weight.
8. polyurethane grouting material according to claim 1, it is characterized in that step a) temperature of reaction be 75～85 ℃, the reaction times is 2～4 hours, the consumption of catalyzer is 0.1 of reaction raw materials weight～2 ‰; Step b) consumption of tensio-active agent is 0.4～0.7% of performed polymer weight.
9. polyurethane grouting material according to claim 1, the weight percentage that it is characterized in that NCO in the described performed polymer is 15～28%.
10. polyurethane grouting material according to claim 9, the weight percentage that it is characterized in that NCO in the described performed polymer is＞22～28%.
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Cited By (5)
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| CN103756289A (en) * | 2013-12-20 | 2014-04-30 | 河南万里路桥集团有限公司 | Pavement crack pouring 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 |
| CN110684166A (en) * | 2019-09-25 | 2020-01-14 | 广东科朗管道修复技术有限公司 | Foaming grouting agent |
| CN115960589A (en) * | 2021-10-11 | 2023-04-14 | 中国石油化工股份有限公司 | Composition for preparing grouting material for drilling and plugging |
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| CN115960589A (en) * | 2021-10-11 | 2023-04-14 | 中国石油化工股份有限公司 | Composition for preparing grouting material for drilling and plugging |
| 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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