CN103756291A - Polyurethane-water glass composite grouting material as well as preparation method and application thereof - Google Patents
Polyurethane-water glass composite grouting material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a polyurethane-water glass composite grouting material as well as a preparation method and an application thereof. The polyurethane-water glass composite grouting material comprises a component A and a component B in a weight ratio of 1:1-1:2, wherein the component A comprises the following components in percentage by weight: 72%-83% of polyurethane prepolymer, 5%-15% of plasticizer, 5%-10% of flame retardant and 2%-3% of surfactant, and the component B comprises the following components in percentage by weight: 99.2%-99.5% of water glass and 0.5%-0.8% of antistatic agent. The obtained composite grouting material has low slurry toxicity and relatively good compressive strength, is dense in jet-grouted solid and does not foam when being wet; and the flame retardancy and the anti-static performance of the composite grouting material meets the requirements of national coal industrial standards MT113-1995; and the polyurethane-water glass composite grouting material can be used for reinforcing coal seams of coal mines.
Description
Technical field
The invention belongs to building material field, be specifically related to a kind of urethane-water glass composite grouting material and preparation method thereof and application.
Background technology
Polyurethanes injection material was developed in Japan the sixties in 20th century, started the eighties to promote in the whole world, was all widely used at present in various buildings, water conservancy, Mineral Engineering.The advantage of polyurethane grouting material has: cohesive force is high, and barrier performance is good; Solidification rate easily regulates, and construction technology, equipment are simple; Meet water reaction fast, can not run off because underground water washes away; Can react with water foaming, produce secondary pressure, thereby pour into more tiny crack; Chemical stability is high, has good weather resistance; Intensity and toughness are better than general chemical grouting material, can process the Special Circumstances such as expansion joint.Meanwhile, because polyurethane grouting material has numerous species, thereby in colliery, there are many different application.More domestic large coal mines, all applied polyurethane grouting material as open a mine Luan Fangezhuang Mine, the red ridge of Henan coalification, Jixi Mining Group etc. of Hebei, had obtained good economic and social benefit.
Oiliness polyurethane grouting material has the features such as intensity is high, weather resistance is strong, is suitable for carrying out coal seam reinforcing, improves the reinforcement operation such as supporting intensity in tunnel, and its application quantity increases just year by year.But also there are some shortcomings and deficiencies in oiliness polyurethane grouting material: pure polyurethane grouting material static resistance deficiency, easily under external influence, produce static, and cause the catastrophic accidents such as gas explosion, fire; In some oiliness polyurethane grouting materials, contain organic solvent, in grouting construction and coal production process, heat can be on fire, adds the flame retardant resistance deficiency of urethane own, causes the intensity of a fire easily to spread, and when burning, can produce hypertoxicity gas, can cause serious secondary disaster; During urethane grouting construction, temperature of reaction is too high, and temperature can reach 120 ℃ even higher, has certain potential safety hazard; In addition, for coal production, coverage is wide, injection material demand is large, but polyurethane grouting material cost is larger, it is per ton 1～20,000 that the price of its basic raw material (isocyanic ester, polyethers) just reaches, and the price of cement, these traditional inorganic grouting materials of water glass is only 1/10th even lower, the therefore expensive popularization that has limited himself of polyurethane grouting material.So colliery polyurethane grouting material is carried out to modification, all significant safely to improving material property and coal production.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of urethane-water glass composite grouting material.
Another object of the present invention is to provide the preparation method of above-mentioned urethane-water glass composite grouting material.
A further object of the present invention is to provide the application of above-mentioned urethane-water glass composite grouting material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of urethane-water glass composite grouting material, is comprised of according to the weight ratio of 1:1～1:2 first component and second component, wherein:
First component comprises following component by weight percentage:
Second component comprises following component by weight percentage:
Water glass 99.2%～99.5%
Static inhibitor 0.5%～0.8%.
Preferably, described in first component, base polyurethane prepolymer for use as is obtained by following preparation method: by polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, polyether glycol, isocyanic ester and Benzoyl chloride after dehydration are added to reactor, stir 10～30min, then in 70～80 ℃ of reactions 2～3 hours, obtain described base polyurethane prepolymer for use as.
Preferred, the weight percent of the polyether glycol after described dehydration is 16.00%～38.64%, and the weight percent of described isocyanic ester is 60.37%～82.04%, and the weight percent of described Benzoyl chloride is 0.99%～1.96%.
Preferred, described polyether glycol is more than one in polyethers N204, polyethers N403 and polyethers 4110c; Described isocyanic ester is diphenylmethanediisocyanate.
Preferred, described churning time is 20min, and described temperature of reaction is 75 ℃; The described reaction times is 2.5 hours.
Preferably, softening agent described in first component is dibutyl phthalate; Described tensio-active agent is the silicone oil SD-502 that hard bubbles; Described fire retardant is tricresyl phosphate (2-chloropropyl) ester or three (2-propyloic) phosphine.
Preferably, water glass described in second component is sodium silicate or potash water glass; Described static inhibitor is stearamide propyl dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate.
The preparation method of above-mentioned urethane-water glass composite grouting material, comprises following steps:
(1) softening agent, fire retardant and tensio-active agent are added base polyurethane prepolymer for use as mix, stir, obtain first component;
(2) water glass and static inhibitor are stirred, obtain second component.
Above-mentioned urethane-water glass composite grouting material is in the application of filling in reinforcing coal pit coal layer, and first component and second component, by weight 1:1～1:2 mix and blend 60～120 seconds, are obtained to urethane-water glass composite grouting material.
Preferably, described churning time is 90 seconds.
Curing mechanism of the present invention: after base polyurethane prepolymer for use as mixes with water glass, in base polyurethane prepolymer for use as-NCO group reacts with the water in water glass, and chain extension, crosslinked produces carbonic acid gas simultaneously; Carbonic acid gas can with water glass in silicate reaction generate unsettled silicic acid, the intermolecular dehydration of silicic acid generates silica network, the stability of water glass colloid also can be destroyed on the other hand; The effect of gel two aspects of the crosslinked and water glass by base polyurethane prepolymer for use as, solidifies system.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention adds water glass to carry out compound grouting on the basis of urethane grouting liquid, can improve flame retardant resistance, the static resistance of oiliness polyurethane grouting material, greatly reduces the cost of polyurethane grouting material simultaneously.
(2) in the present invention, isocyanic ester is prepared as to base polyurethane prepolymer for use as, in utilize in polyether glycol-OH and isocyanic ester-NCO reaction, reduced the content of free-NCO in slurries, slurries toxicity is reduced; And the aggregate of lower-NCO content speed of response when reacting with water glass slows down, and the amount of carbon dioxide producing is less, is conducive to control slurry consolidation speed and suppresses foaming.
(3) the composite grouting material induration that the present invention obtains is closely knit, meets water and does not foam, and has good ultimate compression strength, and flame retardant resistance, antistatic property meet the requirement of state coal industry standard MT113-1995, can be used for coal seam, colliery and reinforces.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 32g polyethers N204,50g diphenylmethanediisocyanate (MDI) and 0.82g Benzoyl chloride, add in container and first mix and blend 10 minutes under cold oil is bathed, then isothermal reaction 3 hours heats up at 80 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent;
(2) preparation of first component
Add softening agent 10g, fire retardant tricresyl phosphate (2-chloropropyl) ester (TCPP) 10g, tensio-active agent 2g to mix base polyurethane prepolymer for use as 78g, stir, obtain first component;
(3) preparation of second component
Sodium silicate 99.2g and static inhibitor 0.8g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:1 mix and blend 120 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Embodiment 2
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 16g polyethers N204,6g polyethers N403,60g diphenylmethanediisocyanate (MDI) and 1.23g Benzoyl chloride, add in container and first mix and blend 20 minutes under cold oil is bathed, then isothermal reaction 2.5 hours heats up at 75 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent.
(2) preparation of first component
Base polyurethane prepolymer for use as 77.5g is added to plasticizer phthalic acid dibutylester (DBP) 15g, fire retardant three (2-propyloic) phosphine (TCEP) 5g and the 2.5g tensio-active agent silicone oil SD-502 that hard bubbles, and mixing and stirring, obtains first component;
(3) preparation of second component
Potash water glass 99.5g and static inhibitor 0.5g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:1 mix and blend 90 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Embodiment 3
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 16g polyethers N204,6g polyethers N403,100g diphenylmethanediisocyanate (MDI) and 1.22g Benzoyl chloride, add in container and first mix and blend 20 minutes under cold oil is bathed, then isothermal reaction 2.5 hours heats up at 75 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent.
(2) preparation of first component
Base polyurethane prepolymer for use as 83g is added to plasticizer phthalic acid dibutylester (DBP) 5g, fire retardant tricresyl phosphate (2-chloropropyl) ester (TCPP) 10g and the 2g tensio-active agent silicone oil SD-502 that hard bubbles, and mixing and stirring, obtains first component;
(3) preparation of second component
Sodium silicate 99.2g and static inhibitor 0.8g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:2 mix and blend 120 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Embodiment 4
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 20g polyethers N204,14g polyethers 4110c, 75g diphenylmethanediisocyanate (MDI) and 2.18g Benzoyl chloride, add in container and first mix and blend 20 minutes under cold oil is bathed, then isothermal reaction 2.5 hours heats up at 75 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent.
(2) preparation of first component
Base polyurethane prepolymer for use as 72g is added to plasticizer phthalic acid dibutylester (DBP) 15g, fire retardant tricresyl phosphate (2-chloropropyl) ester (TCPP) 10g and the 3g tensio-active agent silicone oil SD-502 that hard bubbles, and mixing and stirring, obtains first component;
(3) preparation of second component
Potash water glass 99.5g and static inhibitor 0.5g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:1 mix and blend 90 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Embodiment 5
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 24g polyethers N204,15g polyethers N403,120g diphenylmethanediisocyanate (MDI) and 3.18g Benzoyl chloride, add in container and first mix and blend 30 minutes under cold oil is bathed, then isothermal reaction 2.5 hours heats up at 70 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent.
(2) preparation of first component
Base polyurethane prepolymer for use as 72g is added to plasticizer phthalic acid dibutylester (DBP) 15g, fire retardant tricresyl phosphate (2-chloropropyl) ester (TCPP) 10g and the 3g tensio-active agent silicone oil SD-502 that hard bubbles, and mixing and stirring, obtains first component;
(3) preparation of second component
Sodium silicate 99.5g and static inhibitor 0.5g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:1 mix and blend 90 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Embodiment 6
(1) preparation of base polyurethane prepolymer for use as
By polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, adopt the disposable method feeding intake, by 24g polyethers N204,15g polyethers N403,200g diphenylmethanediisocyanate (MDI) and 4.78g Benzoyl chloride, add in container and first mix and blend 25 minutes under cold oil is bathed, then isothermal reaction 2 hours heats up at 70 ℃, stopped reaction, obtains the base polyurethane prepolymer for use as of light-coloured transparent.
(2) preparation of first component
Base polyurethane prepolymer for use as 77g is added to plasticizer phthalic acid dibutylester (DBP) 10g, fire retardant three (2-propyloic) phosphine (TCEP) 10g and the 3g tensio-active agent silicone oil SD-502 that hard bubbles, and mixing and stirring, obtains first component;
(3) preparation of second component
Potash water glass 99.2g and static inhibitor 0.8g are stirred, obtain second component;
(4) while using, first component, second component, by weight 1:1 mix and blend 90 seconds, are stirred, solidify, obtain urethane-water glass composite grouting material induration.After testing, this urethane-water glass composite grouting material induration flame retardant resistance, antistatic property all meet the requirement of state coal industry standard MT113-1995.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. urethane-water glass composite grouting material, is characterized in that, described urethane-water glass composite grouting material is comprised of according to the weight ratio of 1:1～1:2 first component and second component, wherein:
First component comprises following component by weight percentage:
Second component comprises following component by weight percentage:
Water glass 99.2%～99.5%
Static inhibitor 0.5%～0.8%.
2. urethane-water glass composite grouting material according to claim 1, it is characterized in that, described in first component, base polyurethane prepolymer for use as is obtained by following preparation method: by polyether glycol at 120 ℃, after vacuum tightness 133.3Pa dehydration 2h, polyether glycol, isocyanic ester and Benzoyl chloride after dehydration are added to reactor, stir 10～30min, then in 70～80 ℃ of reactions 2～3 hours, obtain described base polyurethane prepolymer for use as.
3. urethane-water glass composite grouting material according to claim 2, it is characterized in that, the weight percent of the polyether glycol after described dehydration is 16.00%～38.64%, the weight percent of described isocyanic ester is 60.37%～82.04%, and the weight percent of described Benzoyl chloride is 0.99%～1.96%.
4. urethane-water glass composite grouting material according to claim 2, is characterized in that, described polyether glycol is more than one in N204, N403 and polyethers 4110c; Described isocyanic ester is diphenylmethanediisocyanate.
5. urethane-water glass composite grouting material according to claim 2, is characterized in that, described churning time is 20min, and described temperature of reaction is 75 ℃; The described reaction times is 2.5 hours.
6. urethane-water glass composite grouting material according to claim 1, is characterized in that, softening agent described in first component is dibutyl phthalate; Described tensio-active agent is the silicone oil SD-502 that hard bubbles; Described fire retardant is tricresyl phosphate (2-chloropropyl) ester or three (2-propyloic) phosphine.
7. urethane-water glass composite grouting material according to claim 1, is characterized in that, water glass described in second component is sodium silicate or potash water glass; Described static inhibitor is stearamide propyl dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate.
8. the preparation method of the urethane-water glass composite grouting material described in claim 1～7 any one, is characterized in that, comprises following steps:
(1) softening agent, fire retardant and tensio-active agent are added base polyurethane prepolymer for use as mix, stir, obtain first component;
(2) water glass and static inhibitor are stirred, obtain second component.
9. urethane-water glass the composite grouting material described in claim 1～7 any one is in the application of filling in reinforcing coal pit coal layer, it is characterized in that, first component and second component, by weight 1:1～1:2 mix and blend 60～120 seconds, are obtained to urethane-water glass composite grouting material.
10. application according to claim 9, is characterized in that, described churning time is 90 seconds.
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| CN104592485A (en) * | 2015-02-06 | 2015-05-06 | 河南理工大学 | Fire-retardant high-flexibility two-shot grouting material and preparation method thereof |
| CN105111411A (en) * | 2015-05-07 | 2015-12-02 | 山西誉邦科技有限公司 | Epoxy-modified polyurethane-water glass composite grouting material |
| CN105154042A (en) * | 2015-08-28 | 2015-12-16 | 煤炭科学技术研究院有限公司 | Multifunctional additive, preparation method of multifunctional additive and application of multifunctional additive in coal mine reinforcement materials |
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| CN106589283A (en) * | 2016-12-07 | 2017-04-26 | 江苏卓美聚氨酯科技有限公司 | Rigid polyurethane reinforced grouting material and preparation method thereof |
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Application publication date: 20140430 |