CN102911340A - Low-heat-release polyurethane grouting reinforcement material and preparation method thereof - Google Patents
Low-heat-release polyurethane grouting reinforcement material and preparation method thereof Download PDFInfo
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- CN102911340A CN102911340A CN2012103956094A CN201210395609A CN102911340A CN 102911340 A CN102911340 A CN 102911340A CN 2012103956094 A CN2012103956094 A CN 2012103956094A CN 201210395609 A CN201210395609 A CN 201210395609A CN 102911340 A CN102911340 A CN 102911340A
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Abstract
The invention discloses a low-heat-release polyurethane grouting reinforcement material and a preparation method thereof. The low-heat-release polyurethane grouting reinforcement material comprises the following raw materials in parts by mass: 100 parts of polymer polyol, 0.5 to 3.5 parts of amine catalyst, 0.5 to 3.5 parts of tin catalyst, 1 to 4 parts of foam stabilizer, 10 to 50 parts of fire retardant, 50 to 200 parts of adhesive coumarone-indene resin and 100 to 200 parts of isocyanate, wherein the polymer polyol is polyether polyol and/or polyester polyol. The preparation method is simple, the prepared grouting reinforcement material is low in cost and high in curing speed, the reaction heat release temperature is low in the curing process, and the solidification body formed by curing has excellent physical and mechanical properties and is particularly suitable for guaranteeing safety operation under a coal mine.
Description
One, technical field
The present invention relates to a kind of polyurethane material and preparation method thereof, specifically a kind of low heat release urethane slip casting strengthening material and preparation method thereof.
Two, background technology
The urethane injecting paste material has higher compressive strength, excellent adhesive property, and have advantages such as good stability, concrete castability is good, the reaction times is adjustable, thereby be used widely in the grouting and reinforcing field, but when it is applied to Safety of Coal Mine Production as reinforcement material, when being reaction, its shortcoming emits a large amount of heat, and thermal conductivity own is low, heat constantly gathers at material internal, material exothermic heat of reaction excess Temperature, there is serious potential safety hazard, adds that itself cost is higher, therefore greatly limited its range of application.
Three, summary of the invention
The present invention aims to provide a kind of low heat release urethane slip casting strengthening material and preparation method thereof, and technical problem to be solved is to reduce the exothermic temperature of urethane injecting paste material and reduce its thermal discharge, and makes its good mechanical performance, and raw materials cost is cheap.
The present invention hangs down heat release urethane slip casting strengthening material, it is characterized in that its raw material constitutes by mass fraction:
100 parts of polymer polyatomic alcohols, amines catalyst 0.5-3.5 part, tin class catalyzer 0.5-3.5 part, suds-stabilizing agent 1-4 part, fire retardant 10-50 part, additive coumarone-indene resin 50-200 part, isocyanic ester 100-200 part;
Described polymer polyatomic alcohol is polyether glycol and/or polyester polyol.
The functionality of described polyether glycol is 2-6, and molecular weight is 100-2000, viscosity 100-1000mPas;
The functionality of described polyester polyol is 2-4, and molecular weight is 200-3000, viscosity 500-2000mPas.
Described isocyanic ester is many methyl polyphenyl polyisocyanate, reddish-brown viscous liquid ,-NCO content 30-32wt%.
Described amines catalyst is selected from N, N '-dimethylcyclohexylamine, three vinylidene diamines, N, N, N', N', N " one or more in the five methyl diethylentriamine;
Described tin class catalyzer is selected from stannous octoate or dibutyl tin laurate.
Described suds-stabilizing agent is silicone oil, is specially silicone oil AK-8805, is the non-hydrolysis-type polysiloxane-polyether copolymer of a kind of silicon-carbon bond.
Described fire retardant is selected from one or more in ammonium polyphosphate, trichloroethyl phosphate, aluminium hydroxide, the dimethyl methyl phosphonate.
The present invention hangs down the preparation method of heat release urethane slip casting strengthening material, comprises preparation and each unit process of two fluid grouting of pre-treatment, two components:
Described pre-treatment be with polymer polyatomic alcohol at 110-120 ℃ of vacuum-drying 1-2 hour, it is for subsequent use to be cooled to after the room temperature sealing;
The preparation of described pair of component is that pretreated polymer polyatomic alcohol is mixed, and then adds successively amines catalyst, tin class catalyzer, suds-stabilizing agent, fire retardant and additive coumarone-indene resin, obtains component A after stirring; Isocyanic ester is component B;
Described two fluid grouting is to utilize Double-liquid mud-injection pump that component A and B component are injected the ground crack that needs reinforcement, set time 25-150s.
In the two fluid grouting process, coutroi velocity makes component A and component B mix slip casting with the volume ratio of 3:1.
The present invention adds the additive coumarone-indene resin in reaction system, be used for the heat that dispersion and diluting reaction discharge.Employed additive coumarone-indene resin is the low viscosity fluent meterial, and is cheap and easy to get, nontoxic non-volatile.Coumarone-indene resin as inert additwe adding system after, system viscosity reduces, concrete castability is improved, and after polyurethane reaction solidified, intermolecular distance increased, thermal diffusivity is improved, the dilution that is dispersed of the heat that discharges of reaction, heat is difficult to accumulation, thus the core temperature when having reduced polyurethane material reaction curing, meanwhile, cost reduces greatly.
Catalyzer among the present invention is amine and tin class composite catalyst, and amine tin class catalyst ratio is different, and polyurethane reaction set time is different, and adjustable extent set time of reinforcement material of the present invention is 25 ~ 150s.
The concrete preparation process of the present invention is as follows:
1, pre-treatment
With polymer polyatomic alcohol in 110 ~ 120 ℃ of lower vacuum-dryings 1 ~ 2 hour, because of the polymer polyatomic alcohol ratio be easier to the suction, so answer sealed storage after drying is finished.
2, the preparation of component A
Pretreated polymer polyatomic alcohol is mixed, add successively amines catalyst, tin class catalyzer, suds-stabilizing agent and fire retardant, start agitator, fully stirring is uniformly dispersed it, adds coumarone-indene resin again, obtains component A after mixing.
3, the preparation of component B
Component B is isocyanic ester, and selected isocyanic ester is many many methyl of phenyl polyisocyanates (PAPI), isocyano-content 30-32%, functionality 2.7-2.8.
4, solidify
The ratio of 3:1 is got component A and component B by volume, fully stirs it is mixed, and then is poured in the mould and solidifies.
5, sample preparation
After slurry reaction curing is finished, induration to be taken out from mould, room temperature is placed 3d, utilize standard hacksaw and cut-off knife, select its cured article without the epidermis part, avoid bubble, crack, area of stress concentration and be cut into blockly with measured compressed intensity, the batten shape is to survey tensile strength.
6, performance test
Survey its performance according to " colliery reinforcing coal rock mass macromolecular material " industry standard.
7, mixed construction
During site operation, component A and component B are annotated respectively in two charging baskets of two-pack type high-pressure grouting machine, utilize the volume ratio of control valve control component A and component B to be 3:1, utilize high-pressure grouting machine that two component slurries are sprayed in the grouting hole of having accomplished fluently, mix slip casting.After finishing, slip casting utilize organic solvent to clean grout machine.
The present invention has following characteristics:
1, low viscosity.Viscosity of material of the present invention is very low, and component A and component B viscosity have the well property annotated all less than 500mPas, is fit to coal and rock grouting process under the coal mine;
2, low exothermicity.Material cured reaction process exothermic temperature of the present invention is less than 100 ℃, and exothermic temperature is low, is particularly suitable for the processing that coal and rock is reinforced under the coal mine, satisfies the security requirement of using under the coal mine;
3, environmental protection.Material of the present invention does not use the volatile organic solvent, and flash-point is high, and is nontoxic, to the mankind and environmental friendliness;
4, compressive strength is better.Material of the present invention compressive strength after curing is better, can reach 7 ~ 15MPa, satisfies the basic demand of reinforcing fractured coal and rock under the coal mine;
5, high-adhesion.Cohesiveness is good after material gel of the present invention solidifies and between the coal and rock of crack, and the induration of formation has certain elasticity, can satisfy the deformation requirement of various grounds;
6, set time is adjustable.According to field condition, can regulate 25 ~ 150s set time, can adapt to the processing of various complex-terrains;
7, cost is lower.The interpolation of coumarone-indene resin can significantly reduce the cost of raw material.
The present invention compared with prior art has following advantage:
1, because the present invention has used cheap coumarone-indene resin to be raw material in a large number, so that the production cost of material reduces greatly, overcomes the expensive shortcoming of urethane reinforcement material, for such material preparation and application provide very large space.
2, the adding of coumarone-indene resin, so that the exothermic heat of reaction temperature that slurries produce in consolidation process reduces, maximum temperature is below 100 ℃.After this mainly has benefited from adding coumarone-indene resin, the dilution so that the heat that discharges in the polyurethane material solidify reaction process is dispersed, heat is difficult to accumulation, thereby has reduced the exothermic heat of reaction temperature of material.
3, the low property annotated of the slurry viscosity of gained is good among the present invention, and induration good mechanical properties, flame retardant properties are good, and raw material preparation technology and required production and construction equipment are simple, are easy to promote the use of.The set time of injection material of the present invention is adjustable from 25 ~ 150s, the compressive strength of induration can reach 7 ~ 15MPa after slurries solidified, and ageing resistance is good, flame retardant properties good (certainly putting out from fire), and the slurries flash-point is lower than 100 ℃, and fixed thing and cinder adhesive property are good.
Four, embodiment
All reagent of the present invention and raw material are commercial.
Embodiment 1:
(1) with polyether glycol 303(functionality 3, molecular weight 350, viscosity 350 ~ 550mPas) and polyester polyol PF-2011(functionality 2.4, molecular weight 500, viscosity 1000mPas) places vacuum drying oven, 120 ℃ of dry 1.5h, sealed storage after drying is finished.
When (2) treating that the polyethers temperature is reduced to room temperature (25 ℃) left and right sides, take by weighing respectively 40 parts (by weight, down together) polyether glycol 303 and 60 parts of polyester polyol PF-2011 place drying receptacle, take by weighing successively again 0.5 part of dibutyl tin laurate (DBTDL), 0.5 the alcoholic solution (A33) of part three vinylidene diamines, 2 parts of suds-stabilizing agent silicone oil AK-8805,10 parts of dimethyl methyl phosphonates (DMMP), 200 parts of coumarone-indene resins, stir 40s with glass stick and be uniformly dispersed to each component, get component A.
(3) take by weighing 102 parts of polyisocyanates (PAPI), get component B.
(4) with component A and component B by volume the ratio mixing and stirring of 3:1 pour self-vulcanizing in molding jig into until blushing occurs, solidify rear taking-up sample fully until it, place laggard line correlation performance test in three days.
The performance of the urethane slip casting strengthening material that present embodiment prepares is as follows:
Embodiment 2:
(1) with polyether glycol 4110(functionality 4, molecular weight 500, viscosity 3500 ~ 4500mPas) and polyether glycol 303(functionality 3, molecular weight 350, viscosity 350 ~ 550mPas) all places vacuum drying oven, and 120 ℃ of dry 1.5h answer sealed storage after drying is finished.
When (2) treating that the polyethers temperature is reduced to room temperature (25 ℃) left and right sides, take by weighing respectively 30 parts of polyether glycols 4110 and 70 parts of polyether glycols 303 place drying receptacle, take by weighing successively again 1 part of dibutyl tin laurate (DBTDL), the alcoholic solution of 1 part of three vinylidene diamines (A33), 2 parts of suds-stabilizing agent silicone oil AK-8805,10 parts of dimethyl methyl phosphonates (DMMP), 200 parts of coumarone-indene resins, stir 40s with glass stick and be uniformly dispersed to each component, get component A.
(3) take by weighing 135 parts of polyisocyanates PAPI, get component B.
(4) with component A and component B by volume the ratio mixing and stirring of 3:1 pour self-vulcanizing in molding jig into until blushing occurs, solidify rear taking-up sample fully until it, place laggard line correlation performance test in three days.
The performance of the urethane slip casting strengthening material that present embodiment prepares is as follows:
Embodiment 3:
(1) with polyether glycol 4110(functionality 4, molecular weight 500, viscosity 3500 ~ 4500mPas) and aromatic polyester polyol PF-2011(functionality 2.4, molecular weight 500, viscosity 1000mPas) all place vacuum drying oven, 120 ℃ of dry 1.5h answer sealed storage after drying is finished.
When (2) treating that the polyethers temperature is reduced to room temperature (25 ℃) left and right sides, take by weighing respectively 30 parts of polyether glycols 4110 and 70 parts of aromatic polyester polyol PF-2011 place drying receptacle, take by weighing successively again 0.5 part of dibutyl tin laurate (DBTDL), 0.5 the alcoholic solution (A33) of part three vinylidene diamines, 2 parts of suds-stabilizing agent silicone oil AK-8805,7 parts of dimethyl methyl phosphonates, 3 parts of trichloroethyl phosphates, 200 parts of coumarone-indene resins, stir 40s with glass stick and be uniformly dispersed to each component, get reinforcement material component A.
(3) take by weighing 93 parts of polyisocyanates PAPI, get the reinforcement material B component.
(4) with component A and component B by volume the ratio mixing and stirring of 3:1 pour self-vulcanizing in molding jig into until blushing occurs, solidify rear taking-up sample fully until it, place laggard line correlation performance test in three days.
The performance of the urethane slip casting strengthening material that present embodiment prepares is as follows:
Embodiment 4:
(1) with polyether glycol 303(functionality 3, molecular weight 350, viscosity 350 ~ 550mPas) and polyether glycol 330(functionality 3, molecular weight 3000, viscosity 500 ~ 700mPas) all places vacuum drying oven, and 120 ℃ of dry 1.5h answer sealed storage after drying is finished.
When (2) treating that the polyethers temperature is reduced to room temperature (25 ℃) left and right sides, take by weighing respectively 70 parts of polyether glycols 303 and 30 parts of polyether glycols 330 place drying receptacle, take by weighing successively again 1 part of dibutyl tin laurate (DBTDL), the alcoholic solution of 1 part of three vinylidene diamines (A33), 2 parts of suds-stabilizing agent silicone oil AK-8805,10 parts of DMMP, 150 parts of coumarone-indene resins, stir 40s with glass stick and be uniformly dispersed to each component, get reinforcement material component A.
(3) take by weighing 102 parts of polyisocyanates PAPI, get the reinforcement material B component.
(4) with component A and component B by volume the ratio mixing and stirring of 3:1 pour self-vulcanizing in molding jig into until blushing occurs, solidify rear taking-up sample fully until it, place laggard line correlation performance test in three days.
The performance of the urethane slip casting strengthening material that present embodiment prepares is as follows:
Embodiment 5:
(1) with polyether glycol 303(functionality 3, molecular weight 350, viscosity 350 ~ 550mPas) places vacuum drying oven, and 120 ℃ of dry 1.5h answer sealed storage after drying is finished.
When (2) treating that the polyethers temperature is reduced to room temperature (25 ℃) left and right sides, take by weighing 100 parts of polyether glycols 303 and place drying receptacle, take by weighing successively again 3 parts of dibutyl tin laurates (DBTDL), the alcoholic solution of 3 part of three vinylidene diamines (A33), 2 parts of suds-stabilizing agent silicone oil AK-8805,10 parts of DMMP, 200 parts of coumarone-indene resins, stir 40s with glass stick and be uniformly dispersed to each component, get reinforcement material component A.
(3) take by weighing 138 parts of polyisocyanates PAPI, get the reinforcement material B component.
(4) with component A and component B by volume the ratio mixing and stirring of 3:1 pour self-vulcanizing in molding jig into until blushing occurs, solidify rear taking-up sample fully until it, place laggard line correlation performance test in three days.
The performance of the urethane slip casting strengthening material that present embodiment prepares is as follows:
Claims (8)
1. one kind low heat release urethane slip casting strengthening material is characterized in that its raw material constitutes by mass fraction:
100 parts of polymer polyatomic alcohols, amines catalyst 0.5-3.5 part, tin class catalyzer 0.5-3.5 part, suds-stabilizing agent 1-4 part, fire retardant 10-50 part, additive coumarone-indene resin 50-200 part, isocyanic ester 100-200 part;
Described polymer polyatomic alcohol is polyether glycol and/or polyester polyol.
2. low heat release urethane slip casting strengthening material according to claim 1 is characterized in that:
The functionality of described polyether glycol is 2-6, and molecular weight is 100-2000, viscosity 100-1000mPas;
The functionality of described polyester polyol is 2-4, and molecular weight is 200-3000, viscosity 500-2000mPas.
3. low heat release urethane slip casting strengthening material according to claim 1 is characterized in that:
Described isocyanic ester is many methyl polyphenyl polyisocyanate ,-NCO content 30-32%.
4. low heat release urethane slip casting strengthening material according to claim 1 is characterized in that:
Described amines catalyst is selected from N, N '-dimethylcyclohexylamine, three vinylidene diamines, N, N, N', N', N " one or more in the five methyl diethylentriamine;
Described tin class catalyzer is selected from stannous octoate or dibutyl tin laurate.
5. low heat release urethane slip casting strengthening material according to claim 1 is characterized in that:
Described suds-stabilizing agent is silicone oil.
6. low heat release urethane slip casting strengthening material according to claim 1 is characterized in that:
Described fire retardant is selected from one or more in ammonium polyphosphate, trichloroethyl phosphate, aluminium hydroxide, the dimethyl methyl phosphonate.
7. the preparation method of a low heat release urethane slip casting strengthening material claimed in claim 1 comprises it is characterized in that preparation and each unit process of two fluid grouting of pre-treatment, two components:
Described pre-treatment be with polymer polyatomic alcohol at 110-120 ℃ of vacuum-drying 1-2 hour, it is for subsequent use to be cooled to after the room temperature sealing;
The preparation of described pair of component is that pretreated polymer polyatomic alcohol is mixed, and then adds successively amines catalyst, tin class catalyzer, suds-stabilizing agent, fire retardant and additive coumarone-indene resin, obtains component A after stirring; Isocyanic ester is component B;
Described two fluid grouting is to utilize Double-liquid mud-injection pump that component A and B component are injected the ground crack that needs reinforcement, set time 25-150s.
8. preparation method according to claim 7 is characterized in that:
In the two fluid grouting process, coutroi velocity makes component A and component B mix slip casting with the volume ratio of 3:1.
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| CN103254880A (en) * | 2013-03-07 | 2013-08-21 | 河南煤业化工集团研究院有限责任公司 | Gas-extraction hole-sealing material |
| CN106496517A (en) * | 2016-10-09 | 2017-03-15 | 山东大学 | A kind of macromolecule slip casting strengthening material |
| CN109021204A (en) * | 2018-08-17 | 2018-12-18 | 北京瑞诺安科新能源技术有限公司 | A kind of low-heat type polyurethane consolidation by grouting material |
| CN109111726A (en) * | 2017-06-22 | 2019-01-01 | 神华集团有限责任公司 | Composite material and preparation method |
| CN109180893A (en) * | 2018-08-14 | 2019-01-11 | 山东科技大学 | Grouting low heat value high-strength polyurethane material and preparation method thereof |
| CN109608615A (en) * | 2018-12-13 | 2019-04-12 | 长安大学 | A kind of novel oiliness polyurethane slurries and preparation method thereof |
| CN111072894A (en) * | 2019-12-13 | 2020-04-28 | 南通市裕如工程材料有限责任公司 | Polyurethane grouting material and preparation method thereof |
| CN111268941A (en) * | 2019-05-03 | 2020-06-12 | 石家庄国盛矿业科技有限公司 | Novel organic polymer double-liquid type grouting material for coal mine reinforcing coal rock mass |
| CN112194770A (en) * | 2020-10-12 | 2021-01-08 | 煤炭科学技术研究院有限公司 | Functionalized UIO-66/polyurethane composite grouting reinforcing agent and preparation method thereof |
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