CN105294977A - High-strength high-fire-retardant low-heat-release mining polyurethane grouting reinforcement material and preparation method and application thereof - Google Patents
High-strength high-fire-retardant low-heat-release mining polyurethane grouting reinforcement material and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
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Abstract
The invention belongs to the technical field of coal and rock chemical grouting reinforcement, and discloses a high-strength high-fire-retardant low-heat-release mining polyurethane grouting reinforcement material and a preparation method and application thereof. The material is obtained by matching a component I and a component II according to the volume ratio of one to one; the component I is prepared from, by weight, 70%-95% of isocyanate and 5%-30% of epoxy resin; the component II is prepared from, by weight, 30%-50% of flame retardant polyether polyol 1, 10%-20% of flame retardant polyether polyol 2, 25%-40% of plasticizers, 3%-8% of fire retardants, 2%-5% of curing agents, 0.5%-1% of catalyst, 1%-3% of antistatic agents and 0.5%-1% of foam stabilizer.
Description
Technical field
The invention belongs to coal and rock chemical consolidation technical field, particularly a kind of high-intensity high fires low heat release mine polyurethane slip casting strengthening material and preparation method thereof and application.
Background technology
Due to the singularity in field, colliery, for being applied to the high score subclass slip casting strengthening material of underground coal mine except the requirement of mechanical property aspect, for ensureing the construction safety of down-hole, also require that it should possess the features such as lower exothermic heat of reaction amount and higher flame retardant resistance, but existing coal mine polyurethane grouting and reinforcing class material often cannot meet above all requirements, is in particular in the following aspects simultaneously:
1. temperature of reaction is higher.Regulation in existing mine safety industry standard " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011), the maximum temperature of mining polymer grouting and reinforcing class material answers≤140 DEG C.Although Vehicles Collected from Market exists test result that some products react under finite quantity lower than 140 DEG C, but when it is applied to the slip casting of underground coal mine Practical Project, because grouting amount is larger, slurry material aggregate amount is higher, the heat that urethane slurries produce in solidify reaction process is more, and due to environment relative closure, radiating condition wretched insufficiency, make material internal heat accumulation more, temperature rises very fast, maximum temperature even can reach more than 200 DEG C more than 140 DEG C, be easy to pyrolysis of glowing, produce cigarette or naked light phenomenon, and then cause the serious disaster accident such as coal-mine fire.
2. flame retardant resistance is poor.Although some the grouting and reinforcing series products in market meet the requirement of MT113-1995 " underground mine use polymer product fire retardant, antistatic GENERAL EXPERIMENTATION and decision rule ", but the factors such as the slurry homogeneity of material, construction environment, mechanical means and manual operation must be considered due to practical application, current market product still can not meet service requirements completely, when starch material in use there is temperature of reaction too high and fire-retardant rank deficiency when, be just easy to produce the security incident such as cigarette or naked light.
3. the deficiency of mechanical property aspect.Containing isocyanate group in urethane slip casting strengthening material slurries, it very easily with the H that runs in practice of construction process
2o reacts and generates CO
2gas, make material constantly foaming and expansion in the curing process, the slurry material induration mechanical strength after foaming significantly reduces, and very easily causes the failure of slip casting.In addition due to the generation of a large amount of carbon dioxides, make some crack distributed faults bear the higher swelling pressure, finally cause large-scale overall wall caving, roof fall or pressure rack accident.
Therefore, for overcoming the shortcoming of existing mine polyurethane injecting paste material, it is very necessary for researching and developing the new type mining urethane slip casting strengthening material that a kind of intensity is high, flame retardant resistance is high, exothermic heat of reaction is low.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art with not enough, primary and foremost purpose of the present invention is to provide a kind of high-intensity high to fire low heat release mine polyurethane slip casting strengthening material.
Another object of the present invention is to provide above-mentioned high-intensity high to fire the preparation method of low heat release mine polyurethane slip casting strengthening material.
Another object of the present invention is to provide above-mentioned high-intensity high to fire the application of low heat release mine polyurethane slip casting strengthening material.
Object of the present invention is achieved through the following technical solutions:
A kind of high-intensity high fires low heat release mine polyurethane slip casting strengthening material, described material be by first component and second component by volume 1:1 proportioning obtain;
First component comprises following component by weight percentage:
Isocyanic ester 70.0% ~ 95.0%
Epoxy resin 5.0% ~ 30.0%;
Second component comprises following component by weight percentage:
Described isocyanic ester is diphenylmethanediisocyanate (MDI-50);
Described epoxy resin is bisphenol f type epoxy resin 830S, and its epoxy equivalent (weight) is 165 ~ 175g/eq, and under 25 DEG C of conditions, viscosity is 3300 ~ 4300mPas, hydrolysis chlorine≤0.015%.
Described flame retardant polyether polyol 1 is PuranolRF3774, and its hydroxy radical content is 370 ~ 420mgKOH/g, and biodiversity content is that under 0.15%, 25 DEG C of conditions, viscosity is 50 ~ 300mPas; Described flame retardant polyether polyol 2 is PuranolRF3776, and its hydroxy radical content is 310 ~ 350mgKOH/g, and biodiversity content is that under 0.15%, 25 DEG C of conditions, viscosity is 1500 ~ 3500mPas.
Described softening agent is chlorinated paraffin-42, and its chloride quality is that under 40 ~ 44%, 25 DEG C of conditions, viscosity is 1900 ~ 2500mPas;
Described fire retardant is halogenated phosphate based flame retardant FR-310, its phosphorous quality >=12.0%, chloride quality >=14.0%, and under 25 DEG C of conditions, viscosity is 5 ~ 10mPas;
Described solidifying agent is DMP-30;
Described static inhibitor is liquid static inhibitor JA-10ql, light yellow viscous liquid, and under 25 DEG C of conditions, viscosity is 122.4mPas;
Described catalyzer is the mixture of dibutyl tin laurate (DBTDL) and 33% triethylene diamine solution (A-33), and the two mass ratio is 1:1 ~ 2:1;
Described suds-stabilizing agent is hard polyurethane foam silicone oil SD-502.
Above-mentioned high-intensity high fires the preparation method of low heat release mine polyurethane slip casting strengthening material, comprises following steps:
(1) preparation of first component:
In closed reactor, first add epoxy resin by proportioning, then add isocyanic ester, stir 0.5 ~ 1.0h, obtain first component; Wherein, the consumption of each raw material is by weight percentage: epoxy resin 5.0% ~ 30.0%, isocyanic ester 70.0% ~ 95.0%;
(2) preparation of second component
In closed reactor, add flame retardant polyether polyol 1, flame retardant polyether polyol 2, softening agent, fire retardant, solidifying agent, catalyzer, static inhibitor, suds-stabilizing agent successively, mix, stir 2.0 ~ 3.0h, obtain second component; Wherein, the consumption of each raw material is by weight percentage: flame retardant polyether polyol 130.0% ~ 50.0%, flame retardant polyether polyol 210.0% ~ 20.0%, softening agent 25.0% ~ 40.0%, fire retardant 3.0% ~ 8.0%, catalyzer 0.5% ~ 1.0%, solidifying agent 2.0% ~ 5.0%; Static inhibitor 1.0% ~ 3.0%, suds-stabilizing agent 0.5% ~ 1.0%;
(3) first component and second component are mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.
Above-mentioned high-intensity high fire low heat release mine polyurethane slip casting strengthening material within coal mines coal seam reinforce in application.
The present invention has following advantage and effect relative to prior art:
1, by reducing the content of isocyanic ester in whole system, makes itself and H
2o react release CO
2gas reduces, and can reduce foaming and expand, and improves slurry material induration ultimate compression strength.In addition by introducing the ultimate compression strength that epoxy resin can improve induration in polyurethane system.Both comprehensive actions can increase substantially the ultimate compression strength of mine polyurethane slip casting strengthening material.
2 by adding flame retarding polyether in system, chlorinated paraffin-42, fire retardant can improve its flame retardant properties greatly.
3 add inert plasticizer chlorinated paraffin-42, can effectively make reaction liberated heat be dispersed dilution, and heat is difficult to accumulation; In addition, it is slow that epoxy resin and solidifying agent DMP-30 react comparatively polyurethane reaction, and the reaction liberated heat of whole system is discharged by stages, thus reduces the maximum temperature of material.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
In the embodiment of the present invention, performance index measure according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011) method.
Embodiment 1
(1) preparation of first component
In closed reactor, first add 25.0g bisphenol f type epoxy resin 830S, then add 475.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 500.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 100.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 250.0g softening agent chlorinated paraffin-42, 80.0g fire retardant FR-310, 20.0g solidifying agent DMP-30, catalyzer 10.0g (wherein dibutyl tin laurate (DBTDL) 5.0g, A-335.0g), 30.0g static inhibitor JA-10ql, 10.0g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Embodiment 2
(1) preparation of first component
In closed reactor, first add 50.0g bisphenol f type epoxy resin 830S, then add 450.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 460.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 120.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 280.0g softening agent chlorinated paraffin-42, 65.0g fire retardant FR-310, 25.0g solidifying agent DMP-30, catalyzer 10.0g (wherein dibutyl tin laurate (DBTDL) 5.0g, A-335.0g), 30.0g static inhibitor JA-10ql, 10.0g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Embodiment 3
(1) preparation of first component
In closed reactor, first add 75.0g bisphenol f type epoxy resin 830S, then add 425.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 430.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 140.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 310.0g softening agent chlorinated paraffin-42, 50.0g fire retardant FR-310, 30.0g solidifying agent DMP-30, catalyzer 7.5g (wherein dibutyl tin laurate (DBTDL) 5.0g, A-332.5g), 25.0g static inhibitor JA-10ql, 7.5g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Embodiment 4
(1) preparation of first component
In closed reactor, first add 100.0g bisphenol f type epoxy resin 830S, then add 400.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 380.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 160.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 350.0g softening agent chlorinated paraffin-42, 35.0g fire retardant FR-310, 35.0g solidifying agent DMP-30, catalyzer 7.5g (wherein dibutyl tin laurate (DBTDL) 5.0g, A-332.5g), 25.0g static inhibitor JA-10ql, 7.5g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Embodiment 5
(1) preparation of first component
In closed reactor, first add 125.0g bisphenol f type epoxy resin 830S, then add 375.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 340.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 180.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 380.0g softening agent chlorinated paraffin-42, 30.0g fire retardant FR-310, 40.0g solidifying agent DMP-30, catalyzer 5.0g (wherein dibutyl tin laurate (DBTDL) 2.5g, A-332.5g), 20.0g static inhibitor JA-10ql, 5.0g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Embodiment 6
(1) preparation of first component
In closed reactor, first add 150.0g bisphenol f type epoxy resin 830S, then add 350.0g diphenylmethanediisocyanate (MDI-50), stir 0.5 ~ 1.0h, obtain 500.0g first component.
(2) preparation of second component
In closed reactor, add 300.0g flame retardant polyether polyol PuranolRF3774 (Jiahua Chemicals Inc.) successively, 200.0g flame retardant polyether polyol PuranolRF3776 (Jiahua Chemicals Inc.), 400.0g softening agent chlorinated paraffin-42, 30.0g fire retardant FR-310, 50.0g solidifying agent DMP-30, catalyzer 5.0g (wherein dibutyl tin laurate (DBTDL) 2.5g, A-332.5g), 10.0g static inhibitor JA-10ql, 5.0g suds-stabilizing agent SD-502, stir 2.0 ~ 3.0h, obtain 1000.0g second component.
(3) first, second component is mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.In normal conditions, test maximum temperature, ultimate compression strength, flame retardant properties is carried out according to " colliery reinforcing coal rock mass macromolecular material " (AQ1089-2011).Performance index are in table 1.
Table 1 high-intensity high fires low heat release mine polyurethane slip casting strengthening material performance
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. high-intensity high fires a low heat release mine polyurethane slip casting strengthening material, it is characterized in that: described material be by first component and second component by volume 1:1 proportioning obtain;
First component comprises following component by weight percentage:
Isocyanic ester 70.0% ~ 95.0%
Epoxy resin 5.0% ~ 30.0%;
Second component comprises following component by weight percentage:
2. a kind of high-intensity high according to claim 1 fires low heat release mine polyurethane slip casting strengthening material, it is characterized in that: described isocyanic ester is diphenylmethanediisocyanate;
Described epoxy resin is bisphenol f type epoxy resin 830S, and its epoxy equivalent (weight) is 165 ~ 175g/eq, and under 25 DEG C of conditions, viscosity is 3300 ~ 4300mPas, hydrolysis chlorine≤0.015%.
3. a kind of high-intensity high according to claim 1 fires low heat release mine polyurethane slip casting strengthening material, it is characterized in that: described flame retardant polyether polyol 1 is PuranolRF3774, its hydroxy radical content is 370 ~ 420mgKOH/g, biodiversity content is that under 0.15%, 25 DEG C of conditions, viscosity is 50 ~ 300mPas; Described flame retardant polyether polyol 2 is PuranolRF3776, and its hydroxy radical content is 310 ~ 350mgKOH/g, and biodiversity content is that under 0.15%, 25 DEG C of conditions, viscosity is 1500 ~ 3500mPas.
4. a kind of high-intensity high according to claim 1 fires low heat release mine polyurethane slip casting strengthening material, it is characterized in that: described softening agent is chlorinated paraffin-42, and its chloride quality is that under 40 ~ 44%, 25 DEG C of conditions, viscosity is 1900 ~ 2500mPas;
Described fire retardant is halogenated phosphate based flame retardant FR-310, its phosphorous quality >=12.0%, chloride quality >=14.0%, and under 25 DEG C of conditions, viscosity is 5 ~ 10mPas;
Described solidifying agent is DMP-30;
Described static inhibitor is liquid static inhibitor JA-10ql, light yellow viscous liquid, and under 25 DEG C of conditions, viscosity is 122.4mPas;
Described catalyzer is the mixture of dibutyl tin laurate (DBTDL) and 33% triethylene diamine solution (A-33), and the two mass ratio is 1:1 ~ 2:1;
Described suds-stabilizing agent is hard polyurethane foam silicone oil SD-502.
5. a kind of high-intensity high according to any one of Claims 1 to 4 fires the preparation method of low heat release mine polyurethane slip casting strengthening material, it is characterized in that comprising following steps:
(1) preparation of first component:
In closed reactor, first add epoxy resin by proportioning, then add isocyanic ester, stir 0.5 ~ 1.0h, obtain first component; Wherein, the consumption of each raw material is by weight percentage: epoxy resin 5.0% ~ 30.0%, isocyanic ester 70.0% ~ 95.0%;
(2) preparation of second component
In closed reactor, add flame retardant polyether polyol 1, flame retardant polyether polyol 2, softening agent, fire retardant, solidifying agent, catalyzer, static inhibitor, suds-stabilizing agent successively, mix, stir 2.0 ~ 3.0h, obtain second component; Wherein, the consumption of each raw material is by weight percentage: flame retardant polyether polyol 130.0% ~ 50.0%, flame retardant polyether polyol 210.0% ~ 20.0%, softening agent 25.0% ~ 40.0%, fire retardant 3.0% ~ 8.0%, catalyzer 0.5% ~ 1.0%, solidifying agent 2.0% ~ 5.0%; Static inhibitor 1.0% ~ 3.0%, suds-stabilizing agent 0.5% ~ 1.0%;
(3) first component and second component are mixed according to volume ratio 1:1, obtain high-intensity high and fire low heat release mine polyurethane slip casting strengthening material.
6. a kind of high-intensity high according to any one of Claims 1 to 4 fire low heat release mine polyurethane slip casting strengthening material within coal mines coal seam reinforce in application.
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