CN109180893B - Low-calorific-value high-strength polyurethane material for coal mine grouting and preparation method thereof - Google Patents
Low-calorific-value high-strength polyurethane material for coal mine grouting and preparation method thereof Download PDFInfo
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Abstract
The invention provides a low-calorific-value high-strength polyurethane material for coal mine grouting, which relates to the technical field of coal mine safety materials and comprises a component A, a component B and a component C, wherein the component A is mainly prepared from polyether polyol, inorganic filling aggregate, a foam stabilizer, a tin catalyst, a flame retardant, a phase change additive a and polypropylene fibers; the component B is mainly prepared from polyether polyol and a phase change additive B; and the component C is polymeric MDI. The invention achieves the effect of three-step cooling by adopting the phase-change material with lower melting point through chemical reaction, crystallization loss and phase change, thereby preventing the material from being overhigh in temperature in the using process and eliminating the potential safety hazard in the underground operation process of a coal mine; meanwhile, the problems of low strength, easy cracking and the like of the material are solved; environmental protection, no pollution, high curing speed and simple preparation method.
Description
Technical Field
The invention relates to the technical field of coal mine safety materials, in particular to a low-calorific-value high-strength polyurethane material for coal mine grouting and a preparation method thereof.
Background
At present, in the underground coal mine excavation production process, roof fall and rib spalling caused by broken coal rock bodies easily cause human injury accidents, which are always the technical problems that coal mines cannot avoid, and meanwhile, due to coal spontaneous combustion disasters caused by mine air leakage, the broken coal rock bodies and air leakage channels in the mines need to be filled and reinforced. At present, high polymer materials are mainly used in mine reinforcement and filling, but the internal temperature is overhigh due to the accumulation of reaction heat in the use process, so that internal burning cores and external cracking are caused, and coal spontaneous combustion is possibly caused due to high temperature to cause coal mine fire.
The solution of the problems can be started from the aspects of reducing the reaction heat and increasing the crack resistance of the material, and because the heat generated by the reaction of polyether and polymeric MDI in unit mass is certain, the reaction temperature can be reduced by adopting the endothermic reaction or phase change endothermic reaction by adding an additive; the cracking resistance of the material can be improved by increasing the mechanical property of the material and adding additives to enhance the mechanical property of the material. In recent years, a lot of researchers have made a lot of researches on reducing the reaction heat of the mine polyurethane grouting material, but some defects still exist:
the invention patent with application number 201210123159.3 discloses a self-temperature-limiting polyurethane grouting material and a preparation method thereof, and discloses a method for preparing the same, wherein a self-temperature-limiting additive is added into a polyurethane material, and the heat released by the reaction is reduced to be below the boiling point of the additive by utilizing the vaporization of water and an organic solvent in the additive, but because polymeric MDI has high reaction activity, the addition of water is easy to form a competitive reaction with hydroxyl in polyether polyol to a certain extent, so that the reaction is cooled and heated again, and the effect of cooling cannot be really achieved fundamentally.
The invention patent with application number 201310159575.3 discloses a preparation method of a paraffin/polyurethane solid-solid composite double-phase-change energy storage material, which adopts a paraffin hydrocarbon compound with larger phase-change latent heat as a filler to be compounded with a polyurethane matrix with a phase-change function, so as to achieve the purpose of utilizing the double-phase-change energy storage to reduce the temperature.
The invention patent with application number 201710445555.0, namely a high-molecular grouting reinforcement material for coal mines and a preparation method thereof, discloses a method for preparing a prepolymer from A, B components, wherein hydroxyl and isocyanic acid radical are discharged in advance in a reaction kettle to reduce the reaction curing temperature of the material. Although the method can reduce the reaction heat from the raw materials, the method can affect the polyurethane material to a certain extent, reduce the mechanical property of the material, and the preparation process flow is relatively complex, so that the method is not suitable for large-area popularization and use.
Disclosure of Invention
Aiming at the technical problems, the invention provides a low-calorific-value high-strength polyurethane material for coal mine grouting and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-calorific-value high-strength polyurethane material for coal mine grouting comprises a component A, a component B and a component C, wherein the component A is mainly prepared from polyether polyol, inorganic filling aggregate, a foam stabilizer, a tin catalyst, a flame retardant, a phase change additive a and polypropylene fibers; the component B is mainly prepared from polyether polyol and a phase change additive B; and the component C is polymeric MDI.
Further, the raw materials in parts by weight in each component are as follows: the component A comprises 30-60 parts of polyether polyol, 5-15 parts of inorganic filling aggregate, 5-10 parts of foam stabilizer, 5-10 parts of tin catalyst, 5-10 parts of flame retardant, 5-10 parts of phase change additive a and 10-15 parts of polypropylene fiber; 20-40 parts of polyether polyol and 5-10 parts of phase change additive B in the component B; 50-100 parts of polymeric MDI.
Furthermore, the functionality of the polyether polyol in the component A is 4-8, and the relative molecular weight is 200-3000.
Further, the inorganic filling aggregate in the component A is one or more of stone powder, slag micropowder, fly ash and expanded perlite.
Further, the foam stabilizer in the component A is silicone oil, the tin catalyst is stannous octoate, and the flame retardant is trichloroethyl phosphate.
Furthermore, the polypropylene fiber in the component A is a chopped polypropylene fiber with the length of 3mm and the diameter of 8-13 μm.
Further, the phase change additive a in the component A is aluminum ammonium sulfate dodecahydrate, and the phase change additive B in the component B is barium hydroxide octahydrate.
More preferably, aluminum ammonium sulfate dodecahydrate powder having a melting point of 82.3 ℃, a specific heat capacity of 1.706 kJ/(kg. K) and a salt content of 47.69% is used as the phase change additive a, and barium hydroxide octahydrate powder having a melting point of 78 ℃ is used as the phase change additive b.
Further, the polymeric MDI of the C component is polymethylene polyphenyl isocyanate, and the content of isocyanic acid radical (-NCO) is 28-30%.
The preparation method of the low-calorific-value high-strength polyurethane material for coal mine grouting comprises the following steps:
(1) grinding selected inorganic filling aggregate for multiple times to be nano-grade, then drying for more than two hours at the temperature of 120 ℃, pumping a certain amount of polyether polyol to a mixing kettle, sequentially adding a selected foam stabilizer, a tin catalyst, a flame retardant, ammonium aluminum sulfate dodecahydrate and short-cut polypropylene fibers into the mixing kettle, simultaneously adding a certain amount of dried nano inorganic filling aggregate into the mixing kettle, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping a certain amount of polyether polyol to a mixing kettle by a pump, and adding a certain amount of barium hydroxide octahydrate to the mixing kettle to prepare a component B;
(3) preparation of component C: pumping a certain amount of polymethylene polyphenyl isocyanate to prepare a component C;
(4) and after the materials are mixed, opening a grouting pump, premixing the component A and the component B in a pipeline mixer through the grouting pump, carrying out three-liquid mixing on the component C and the two premixed components in a spray gun, spraying out the mixture through a nozzle, and curing to obtain the low-heat high-strength polyurethane material for coal mine grouting.
In the preparation method, the following three cooling processes are mainly realized:
(1) after two phase change additives are added into polyether and fully mixed and stirred, because aluminum ammonium sulfate dodecahydrate and barium hydroxide octahydrate perform endothermic reaction, a part of heat is absorbed, and the first temperature reduction process is performed;
(2) when the polyurethane reaction temperature is raised to the melting points of the two phase-change additives, the two phase-change additives are melted to change phases, so that a part of heat is absorbed, and the second step of cooling process is performed;
(3) the reaction temperature is continuously raised, the crystallization water is continuously lost in the process of the ammonium aluminum sulfate dodecahydrate and the barium hydroxide octahydrate, and the crystallization water is vaporized to absorb the reaction heat again due to the higher temperature, so that the third temperature reduction process is realized.
At present, A, B two components are mostly used as the mining grouting material, the component A mainly comprises polyether polyol and various auxiliaries, the component B mainly comprises polymeric MDI, the component A and the component B are mixed and reacted to form the grouting material, although the performance of the polyurethane material after reaction is excellent, due to the fact that-OH and-NCO have high activity in the using process, a large amount of heat is released under the condition of a catalyst, and the temperature inside the material is too high; based on the point, on the premise of not influencing the material performance, the ammonium aluminum sulfate dodecahydrate and the barium hydroxide octahydrate are respectively added into the polyether for pre-reaction and absorbing heat, and then are mixed with the polymeric MDI, so that the heat generated by the reaction is greatly reduced.
The beneficial effect of the invention is that,
1. aiming at the problem that the polyurethane material has high heat in the underground application process and is likely to cause coal mine fire, the phase-change material with lower melting point is adopted to achieve the effect of three-step cooling through chemical reaction, crystallization loss and phase change, so that the fire caused by high temperature in the use process of the material is prevented, and the potential safety hazard in the underground operation process of the coal mine is eliminated;
2. the addition of the polypropylene fiber realizes further optimization of the mechanical property of the solidified body, and solves the problems of low strength, easy cracking and the like of the material;
3. the problems of large change of expansion with heat and contraction with cold, inaccurate knot top and loose wind plugging caused by high reaction temperature are solved;
4. has the advantages of environmental protection, no pollution, high curing speed, simple preparation method, low price of raw materials and wide application prospect.
Drawings
FIG. 1 is a schematic view of a process for preparing the present invention;
in the figure: 1. a container I; 2. a container II; 3. a container III; 4. a mixing kettle I; 5. a mixing kettle II; 6. grouting pump; 7. a pipeline mixer; 8. a spray gun; 9. and (4) a nozzle.
Detailed Description
Example 1
A low-calorific-value high-strength polyurethane material for coal mine grouting is shown in figure 1 and is prepared by the following steps:
(1) preparation of component A: grinding 5 parts of slag micro powder for multiple times to a nano level, and then drying for more than two hours at 120 ℃; pumping 30 parts of polyether polyol (with functionality of 4 and relative molecular weight of 1000) in a container I1 to a mixing kettle I4 through a pump, sequentially adding 5 parts of silicone oil, 5 parts of stannous octoate, 5 parts of trichloroethyl phosphate, 5 parts of ammonium aluminum sulfate dodecahydrate and 10 parts of chopped polypropylene fibers (with the length of 3mm and the diameter of 8 mu m) into the mixing kettle I4, simultaneously adding 5 parts of dried nano slag micro powder into the mixing kettle I4, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping 20 parts of polyether polyol in the container II 2 to a mixing kettle II 5 by a pump, and adding 5 parts of barium hydroxide octahydrate to the mixing kettle II 5 to prepare a component B;
(3) preparation of component C: pumping 50 parts of polymethylene polyphenyl isocyanate in a container III 3 by a pump to prepare a component C;
(4) and after the materials are mixed, the grouting pump 6 is opened, the component A and the component B are premixed in a pipeline mixer 7 through the grouting pump 6, the component C and the two premixed components are subjected to three-liquid mixing in a spray gun 8, and are sprayed out through a nozzle 9 and cured to obtain the low-heat high-strength polyurethane material for coal mine grouting. The performance test results of the low-heat value high-strength polyurethane material prepared in the example are shown in table one:
TABLE-Low calorific value high-strength polyurethane material properties
| Performance of | Index (I) |
| Curing time(s) | 35 |
| Endothermic reaction (J/g) | 62.2 |
| Latent heat of fusion (J/g) | 103.4 |
| Latent heat of vaporization (J/g) | 48 |
| Maximum reaction temperature (. degree.C.) | 88 |
| Compressive strength (MPa) | 48 |
Example 2
A low-calorific-value high-strength polyurethane material for coal mine grouting is shown in figure 1 and is prepared by the following steps:
(1) preparation of component A: grinding 15 parts of stone powder for multiple times to a nano level, drying for more than two hours at 120 ℃, pumping 60 parts of polyether polyol (with functionality of 4 and relative molecular weight of 1000) in a container I1 to a mixing kettle I4, sequentially adding 10 parts of silicone oil, 10 parts of stannous octoate, 10 parts of trichloroethyl phosphate, 10 parts of ammonium aluminum sulfate dodecahydrate and 15 parts of chopped polypropylene fibers (with length of 3mm and diameter of 10 mu m) into the mixing kettle I4, simultaneously adding 15 parts of dried nano stone powder into the mixing kettle I4, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping 40 parts of polyether polyol in a container II 2 to a mixing kettle II 5 by a pump, and adding 10 parts of barium hydroxide octahydrate to the mixing kettle II 5 to prepare a component B;
(3) preparation of component C: pumping 100 parts of polymethylene polyphenyl isocyanate in a container III 3 to prepare a component C;
(4) and after the materials are mixed, the grouting pump 6 is opened, the component A and the component B are premixed in a pipeline mixer 7 through the grouting pump 6, the component C and the two premixed components are subjected to three-liquid mixing in a spray gun 8, and are sprayed out through a nozzle 9 and cured to obtain the low-heat high-strength polyurethane material for coal mine grouting. The performance test results of the low-heat-value high-strength polyurethane material prepared in the example are shown in the table two:
TABLE II low heat value high strength polyurethane material performance
| Performance of | Index (I) |
| Curing time(s) | 37 |
| Endothermic reaction (J/g) | 70.2 |
| Latent heat of fusion (J/g) | 115.4 |
| Latent heat of vaporization (J/g) | 51 |
| Maximum reaction temperature (. degree.C.) | 93 |
| Compressive strength (MPa) | 57 |
Example 3
A low-calorific-value high-strength polyurethane material for coal mine grouting is shown in figure 1 and is prepared by the following steps:
(1) preparation of component A: grinding 10 parts of fly ash for multiple times to a nano level, drying for more than two hours at 120 ℃ for later use, pumping 35 parts of polyether polyol (with functionality of 4 and relative molecular weight of 1000) in a container I1 to a mixing kettle I4 through a pump, sequentially adding 5 parts of silicone oil, 5 parts of stannous octoate, 5 parts of trichloroethyl phosphate, 5 parts of ammonium aluminum sulfate dodecahydrate and 10 parts of chopped polypropylene fibers (with the length of 3mm and the diameter of 9 mu m) into the mixing kettle I4, simultaneously adding 10 parts of dried nano fly ash into the mixing kettle I4, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping 25 parts of polyether polyol in the container II 2 to a mixing kettle II 5 by a pump, and adding 5 parts of barium hydroxide octahydrate to the mixing kettle II 5 to prepare a component B;
(3) preparation of component C: pumping 60 parts of polymethylene polyphenyl isocyanate in a container III 3 to prepare a component C;
(4) and after the materials are mixed, opening a grouting pump 6, premixing the component A and the component B in a pipeline mixer 7 through the grouting pump 6, carrying out three-liquid mixing on the component C and the two premixed components in a spray gun 8, spraying out the mixture through a nozzle 9, and curing to obtain the low-heat high-strength polyurethane material for coal mine grouting. The performance test results of the low-heat-value high-strength polyurethane material prepared in the example are shown in table three:
performance of high-strength polyurethane material with low heat value
| Performance of | Index (I) |
| Curing time(s) | 43 |
| Endothermic reaction (J/g) | 72.5 |
| Latent heat of fusion (J/g) | 118.1 |
| Latent heat of vaporization (J/g) | 47 |
| Maximum reaction temperature (. degree.C.) | 95 |
| Compressive strength (MPa) | 57.3 |
Example 4
A low-calorific-value high-strength polyurethane material for coal mine grouting is shown in figure 1 and is prepared by the following steps:
(1) preparation of component A: grinding 8 parts of expanded perlite for multiple times to a nano level, drying for more than two hours at 120 ℃ for later use, pumping 42 parts of polyether polyol (with functionality of 4 and relative molecular weight of 1000) in a container I1 to a mixing kettle I4, sequentially adding 7 parts of silicone oil, 7 parts of stannous octoate, 7 parts of trichloroethyl phosphate, 7 parts of ammonium aluminum sulfate dodecahydrate and 12 parts of chopped polypropylene fiber (with length of 3mm and diameter of 12 mu m) into the mixing kettle I4, simultaneously adding 8 parts of dried nano expanded perlite into the mixing kettle I4, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping 33 parts of polyether polyol in a container II 2 to a mixing kettle II 5 by a pump, and adding 7 parts of barium hydroxide octahydrate to the mixing kettle II 5 to prepare a component B;
(3) preparation of component C: pumping 75 parts of polymethylene polyphenyl isocyanate in a container III 3 to prepare a component C;
(4) and after the materials are mixed, the grouting pump 6 is opened, the component A and the component B are premixed in a pipeline mixer 7 through the grouting pump 6, the component C and the two premixed components are subjected to three-liquid mixing in a spray gun 8, and are sprayed out through a nozzle 9 and cured to obtain the low-heat high-strength polyurethane material for coal mine grouting. The performance test results of the low-heat value high-strength polyurethane material prepared in the example are shown in table four:
TABLE IV Low calorific value high strength polyurethane Material Properties
| Performance of | Index (I) |
| Curing time(s) | 46 |
| Endothermic reaction (J/g) | 88.5 |
| Latent heat of fusion (J/g) | 116.8 |
| Latent heat of vaporization (J/g) | 51 |
| Maximum reaction temperature (. degree.C.) | 79 |
| Compressive strength (MPa) | 63 |
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.
Claims (7)
1. The low-calorific-value high-strength polyurethane material for coal mine grouting is characterized by comprising a component A, a component B and a component C, wherein the component A is mainly prepared from polyether polyol, inorganic filling aggregate, a foam stabilizer, a tin catalyst, a flame retardant, a phase change additive a and polypropylene fibers; the component B is mainly prepared from polyether polyol and a phase change additive B; the component C is polymeric MDI; the raw materials in the components in parts by weight are as follows: the component A comprises 30-60 parts of polyether polyol, 5-15 parts of inorganic filling aggregate, 5-10 parts of foam stabilizer, 5-10 parts of tin catalyst, 5-10 parts of flame retardant, 5-10 parts of phase change additive a and 10-15 parts of polypropylene fiber; 20-40 parts of polyether polyol and 5-10 parts of phase change additive B in the component B; 50-100 parts of polymeric MDI; the phase change additive a in the component A is aluminum ammonium sulfate dodecahydrate, and the phase change additive B in the component B is barium hydroxide octahydrate.
2. The low-calorific-value high-strength polyurethane material for coal mine grouting according to claim 1, wherein the polyether polyol in the component A has a functionality of 4 to 8 and a relative molecular weight of 200 to 3000.
3. The low-calorific-value high-strength polyurethane material for coal mine grouting according to claim 1, wherein the inorganic filling aggregate in the component A is one or more of stone powder, slag micropowder, fly ash and expanded perlite.
4. The low-calorific-value high-strength polyurethane material for coal mine grouting according to claim 1, wherein the foam stabilizer in the component A is silicone oil, the tin catalyst is stannous octoate, and the flame retardant is trichloroethyl phosphate.
5. The low-calorific-value high-strength polyurethane material for coal mine grouting according to claim 1, wherein the polypropylene fibers in the component A are chopped polypropylene fibers with the length of 3mm and the diameter of 8-13 μm.
6. A low calorific value high strength polyurethane material for coal mine grouting according to claim 1, wherein the polymeric MDI of the C-component is polymethylene polyphenyl isocyanate and has an isocyanate group (-NCO) content of 30.5% to 32.0%.
7. The preparation method of the low-heat-value high-strength polyurethane material for coal mine grouting according to any one of claims 1 to 6, characterized by comprising the following steps:
(1) preparation of component A: grinding selected inorganic filling aggregate for multiple times to be nano-grade, then drying for more than two hours at the temperature of 120 ℃, pumping 30-60 parts of polyether polyol to a mixing kettle through a pump, sequentially adding selected foam stabilizer, tin catalyst, flame retardant, ammonium aluminum sulfate dodecahydrate and chopped polypropylene fiber into the mixing kettle, simultaneously adding 5-15 parts of dried nano inorganic filling aggregate into the mixing kettle, and fully stirring to prepare a component A;
(2) preparation of the component B: pumping 20-40 parts of polyether polyol to a mixing kettle by a pump, and adding 5-10 parts of barium hydroxide octahydrate to the mixing kettle to prepare a component B;
(3) preparation of component C: pumping 50-100 parts of polymethylene polyphenyl isocyanate by a pump to prepare a component C;
(4) and after the ingredients are mixed, opening a grouting pump, premixing the component A and the component B in a pipeline mixer through the grouting pump, carrying out three-liquid mixing on the component C and the two premixed components in a spray gun, spraying out the mixture through a nozzle, and curing to obtain the low-heat-value high-strength polyurethane material for coal mine grouting.
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| CN110183612B (en) * | 2019-05-24 | 2021-09-07 | 山西省交通科技研发有限公司 | Grouting material for quickly repairing underground engineering wall seepage water and preparation method thereof |
| CN111138622A (en) * | 2019-12-31 | 2020-05-12 | 河北浩威旭光新材料科技有限公司 | Organic polymer ultralow-temperature reinforcing material for coal rock mass |
| CN114605607B (en) * | 2022-04-07 | 2023-03-03 | 中国矿业大学 | Phase-change hydrated salt polymerization filling material and preparation method and use method thereof |
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