Ultra-low viscosity grouting material suitable for roadway of coal mine powdery difficult permeable coal body and preparation method thereof

Abstract

The present application provides a kind of super low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway and its preparation method, and the preparation method includes the following steps: weighing class A mixed monomer, class B composite catalyst, class B catalytic promoter, reinforcing agent, antioxidant, flame retardant, heating stirring, to obtain grouting material A material;Weighing class B mixed monomer, class A composite catalyst, class A catalytic promoter, reinforcing agent, antioxidant, flame retardant, heating stirring, uniformly mixed, to obtain grouting material B material.When site grouting reinforcement, grouting material A material is mixed with grouting material B material, so that the two grouting materials solidify, and the stability is enhanced.The grouting material A material prepared by the present application and the grouting material B viscosity are low, the flow resistance is small, can penetrate into the small crack of coal mine roadway surrounding rock and polymerize into macromolecule in situ, the permeability of slurry is improved, the bonding strength of grouting material and coal body interface is improved, and the grouting reinforcement effect is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of coal mine grouting material, and particularly relates to an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway and a preparation method thereof. BACKGROUND

[0002] A coal mine roadway safety and efficient complete support technology based on geomechanics testing and taking anchoring and grouting as cores has been formed in China. Through grouting technology, slurry can be injected into cracks and holes of a coal mine roadway surrounding rock to form a certain consolidated body to enhance the stability of the roadway, the bearing capacity and crack resistance of the coal mine roadway surrounding rock, and the strength and stability of the coal mine roadway surrounding rock space. However, in a coal mine powdery difficult-to-penetrate coal roadway, the grouting material has the problems of large slurry viscosity and difficulty in being injected into a small crack, and the grouting reinforcement has the problems of small slurry consumption, difficulty in slurry penetration, and limited reinforcement effect, which seriously affects the grouting effect and is the most important factor restricting the grouting reinforcement of the coal mine powdery difficult-to-penetrate coal roadway. Therefore, it is urgent to develop an ultra-low viscosity grouting material suitable for the coal mine powdery difficult-to-penetrate coal roadway. SUMMARY

[0003] The present application aims to at least solve one of the problems in the related art. To this end, the present application provides an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway and a preparation method thereof, which can improve the permeability of the grouting material and improve the grouting reinforcement effect.

[0004] An embodiment of the present application provides a preparation method of an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway, which comprises the following steps:

[0005] S1, A type mixed monomers 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 1-5 parts, antioxidant 1-3 parts, and flame retardant 1-2 parts are weighed according to the mass fraction, heated and stirred, uniformly mixed, and a grouting material A material is obtained; wherein the A type mixed monomers include acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, and the mass ratio of the acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0006] S2, B type mixed monomers 100 parts, A type composite catalyst 1-3 parts, A type catalytic promoter 1-2 parts, reinforcing agent 1-5 parts, antioxidant 1-2 parts, and flame retardant 1-3 parts are weighed according to the mass fraction, heated and stirred, uniformly mixed, and a grouting material B material is obtained; wherein the B type mixed monomers include phenylalanine, pyrrole lysine and alanine, and the mass ratio of the phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0007] In some embodiments, the B-type composite catalyst comprises platinum black and palladium powder, and the mass ratio of the platinum black and the palladium powder is 1:3.

[0008] In some embodiments, the B-type catalytic promoter comprises copper bromide and magnesium oxide, and the mass ratio of the copper bromide and the magnesium oxide is 2:1.

[0009] In some embodiments, the A-type composite catalyst comprises cyclotriphosphazene base and 2-imidazolidone, and the mass ratio of the cyclotriphosphazene base and the 2-imidazolidone is 1:1.

[0010] In some embodiments, the A-type catalytic promoter comprises 2-methylimidazole and benzimidazole, and the mass ratio of the 2-methylimidazole and the benzimidazole is 7:1.

[0011] In some embodiments, the reinforcing agent comprises nano calcium carbonate, nano titanium dioxide and nano cesium carbonate, and the mass ratio of the nano calcium carbonate, the nano titanium dioxide and the nano cesium carbonate is 1:9:2.

[0012] In some embodiments, the antioxidant comprises tert-butyl hydroquinone and glutathione, and the mass ratio of the tert-butyl hydroquinone and the glutathione is 4:1.

[0013] In some embodiments, the flame retardant comprises tributyl phosphate, tris(2-ethylhexyl) phosphate and tris(2-chloroethyl) phosphate, and the mass ratio of the tributyl phosphate, the tris(2-ethylhexyl) phosphate and the tris(2-chloroethyl) phosphate is 3:1:1.

[0014] In some embodiments, in the step S1, the heating and stirring is performed at a temperature of 18-22℃ for 55-60 minutes at a stirring speed of 1500 revolutions per minute, and in the step S2, the heating and stirring is performed at a temperature of 18-22℃ for 70-80 minutes.

[0015] Another aspect of the present application provides an ultra-low viscosity grouting material prepared by the above preparation method, which comprises a grouting material A and a grouting material B. In use, the grouting material A and the grouting material B are mixed, the A-type mixed monomers in the grouting material A and the A-type composite catalyst and the A-type catalytic promoter in the grouting material B are subjected to in-situ polymerization reaction, and the B-type mixed monomers in the grouting material B and the B-type composite catalyst and the B-type catalytic promoter in the grouting material A are subjected to in-situ polymerization reaction. BRIEF DESCRIPTION OF DRAWINGS

[0016] The above and / or additional aspects and advantages of the present application will become apparent and be readily understood from the following description, taken in conjunction with the following drawings, in which:

[0017] Wherein:

[0018] Figure 1 The flow chart of the preparation method of the ultra-low viscosity grouting material for the coal mine powdery difficult-to-penetrate coal roadway in the embodiment of the present application. DETAILED DESCRIPTION

[0019] The embodiments of the present application are described in detail below, and examples of the embodiments are shown in the accompanying drawings. The embodiments described below by referring to the accompanying drawings are exemplary and are intended to explain the present application, and cannot be understood as a limitation of the present application.

[0020] The nanofiber-reinforced polyester fiber web material suitable for coal mine soft rock roadway support and the preparation method thereof in the embodiment of the present application are described below with reference to the accompanying drawings.

[0021] As shown in the drawings, Figure 1 The embodiment of the present application proposes a preparation method of an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway, which comprises the following steps:

[0022] S1, A type mixed monomers 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 1-5 parts, antioxidant 1-3 parts, and flame retardant 1-2 parts are weighed according to the mass fraction, heated and stirred, uniformly mixed to obtain grouting material A material; wherein the A type mixed monomers include acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, and the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0023] S2, B type mixed monomers 100 parts, A type composite catalyst 1-3 parts, A type catalytic promoter 1-2 parts, reinforcing agent 1-5 parts, antioxidant 1-2 parts, and flame retardant 1-3 parts are weighed according to the mass fraction, heated and stirred, uniformly mixed to obtain grouting material B material, wherein the B type mixed monomers include phenylalanine, pyrrole lysine and alanine, and the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0024] The grouting material A material and the grouting material B material obtained by the preparation method of the embodiment of the present application are mixed when on-site grouting and reinforcement is performed, the A type mixed monomers in the grouting material A material and the A type composite catalyst and the A type catalytic promoter in the grouting material B material occur in-situ polymerization reaction, the B type mixed monomers in the grouting material B material and the B type composite catalyst and the B type catalytic promoter in the grouting material A material occur in-situ polymerization reaction, the grouting material A material and the grouting material B material are solidified, and the stability is enhanced.

[0025] The prepared grouting material A and grouting material B are polymerized to form functional groups such as hydroxyl groups, amino groups and amide groups, and multiple hydrogen bonds are formed with the hydroxyl groups and carboxyl groups on the surface of the coal body, so that the bonding strength of the grouting material and the coal body interface is improved, and the grouting control effect is improved.

[0026] The prepared grouting material A and grouting material B have low viscosity and small flow resistance, can penetrate into small cracks in the surrounding rock of the coal mine tunnel, and are polymerized into macromolecules in situ, so that the permeability of the grout is improved, and the grouting reinforcement effect is improved.

[0027] The prepared grouting material A and grouting material B are mixed, and the two types of copolymer macromolecules formed by in-situ polymerization are staggered and transmitted to each other to form a polymer interpenetrating network structure, exhibit a mechanical interlocking effect, significantly improve the strength of the grouting material, and improve the grouting reinforcement effect.

[0028] The prepared grouting material A and grouting material B are mixed, and the two types of copolymer macromolecules formed by in-situ polymerization are staggered and transmitted to each other to form a polymer interpenetrating network structure, exhibit a mechanical interlocking effect, significantly improve the strength of the grouting material, and improve the grouting reinforcement effect.

[0029] The preparation method of the embodiment of the present application is simple, low in cost and strong in practicability.

[0030] It should be noted that the ratio of each substance in the A-type mixed monomer and the B-type mixed monomer is limited, and if the amount of a certain monomer is too high or too low, the reaction will not be sufficient, the monomer will be left, and the compressive strength and setting time will be affected.

[0031] Further, when used, the grouting material A and the grouting material B are injected by a double-liquid grouting pump.

[0032] In some embodiments, the B-type composite catalyst includes platinum black and palladium powder, and the mass ratio of the platinum black to the palladium powder is 1:3.

[0033] In some embodiments, the B-type catalytic promoter includes copper bromide and magnesium oxide, and the mass ratio of the copper bromide to the magnesium oxide is 2:1.

[0034] In some embodiments, the A-type composite catalyst includes cyclotriphosphazene base and 2-imidazolidone, and the mass ratio of the cyclotriphosphazene base to the 2-imidazolidone is 1:1.

[0035] In some embodiments, the A-type catalytic promoter includes 2-methylimidazole and benzimidazole, and the mass ratio of the 2-methylimidazole to the benzimidazole is 7:1.

[0036] In some embodiments, the reinforcing agent comprises nano calcium carbonate, nano titanium dioxide and nano cesium carbonate, and the mass ratio of the nano calcium carbonate, the nano titanium dioxide and the nano cesium carbonate is 1:9:2.

[0037] In some embodiments, the antioxidant comprises tert-butyl hydroquinone and glutathione, and the mass ratio of the tert-butyl hydroquinone and the glutathione is 4:1.

[0038] In some embodiments, the flame retardant comprises tributyl phosphate, tris(2-ethylhexyl) phosphate and tris(2-chloroethyl) phosphate, and the mass ratio of the tributyl phosphate, the tris(2-ethylhexyl) phosphate and the tris(2-chloroethyl) phosphate is 3:1:1.

[0039] It should be noted that the reinforcing agent, the antioxidant and the flame retardant in the grouting material A and the grouting material B are the same.

[0040] In some embodiments, in the step S1, the heating and stirring are performed at a temperature of 18-22℃ for 55-60 minutes at a stirring speed of 1500 revolutions per minute, and in the step S2, the heating and stirring are performed at a temperature of 18-22℃ for 70-80 minutes.

[0041] It should be noted that if the temperature is too high, the active groups of the monomers will be damaged, resulting in incomplete reaction; if the temperature is too low, the substances cannot reach the reaction temperature, resulting in that the reaction cannot be performed. Therefore, the reaction temperature is set in the range of 18-22℃. If the range is exceeded, the viscosity of the prepared grouting material will be greatly reduced, and the compressive strength cannot meet the use requirements.

[0042] Another aspect of the embodiments of the present application provides a super-low viscosity grouting material prepared by the preparation method, which comprises a grouting material A and a grouting material B. When used, the grouting material A and the grouting material B are mixed at a ratio of (0.8-1.2):(0.8-1.2), the A-type mixed monomers in the grouting material A and the A-type composite catalyst and the A-type catalytic promoter in the grouting material B perform in-situ polymerization reaction, and the B-type mixed monomers in the grouting material B and the B-type composite catalyst and the B-type catalytic promoter in the grouting material A perform in-situ polymerization reaction.

[0043] The grouting material A and the grouting material B prepared by the embodiments of the present application form functional groups such as hydroxyl groups, amino groups and amide groups after polymerization, and form multiple hydrogen bonds with the hydroxyl groups and the carboxyl groups on the surface of the coal body, so that the bonding strength of the grouting material and the coal body interface is improved, and the grouting control effect is improved.

[0044] The grouting material A and the grouting material B prepared by the embodiments of the present application have low viscosity and small flow resistance, can penetrate into small cracks in the surrounding rock of the coal mine roadway and polymerize into macromolecules in-situ, the permeability of the grouting liquid is improved, and the grouting reinforcement effect is improved.

[0045] The two types of copolymer macromolecules formed by in-situ polymerization after mixing the grouting material A and the grouting material B are interlaced and transmitted to each other, a polymer interpenetrating network structure is formed, a mechanical interlocking effect is presented, the strength of the grouting material is significantly improved, and the reinforcement effect of grouting is improved.

[0046] It should be noted that the mixing ratio of the grouting material A and the grouting material B is limited to (0.8-1.2):(0.8-1.2), because if the ratio is higher than this range, the monomer and the catalyst will be out of balance, the reaction will be too fast, the setting time will be too fast, and then the coal rock body crack will be solidified before the grouting material is injected into the coal rock body crack. If the ratio is lower than this range, the reaction rate will be too slow, and the grouting material will not be solidified for a long time after being injected into the coal rock body crack.

[0047] The application will be further described through specific examples.

[0048] Example 1

[0049] A preparation method of an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway, comprising the following steps:

[0050] S1, 100 parts of A type mixed monomers, 3 parts of B type composite catalyst, 1 part of B type catalytic promoter, 1 part of reinforcing agent, 1 part of antioxidant and 1 part of flame retardant are weighed according to the mass fraction, added to a stirrer, heated to 18℃, stirred for 55 minutes, uniformly mixed, and grouting material A is obtained; wherein the A type mixed monomers include acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, and the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0051] S2, 100 parts of B type mixed monomers, 1 part of A type composite catalyst, 1 part of A type catalytic promoter, 1 part of reinforcing agent, 1 part of antioxidant and 1 part of flame retardant are weighed according to the mass fraction, added to a stirrer, heated to 18℃, stirred for 70 minutes, uniformly mixed, and grouting material B is obtained, wherein the B type mixed monomers include phenylalanine, pyrrole lysine and alanine, and the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0052] When used, the grouting material A and the grouting material B are mixed according to 1:1.

[0053] The viscosity of the grouting material A is 7.5 mPas, the viscosity of the grouting material B is 5.3 mPas, the curing time of the mixed grouting material A and grouting material B is 67 s, and the compressive strength after curing is 49 MPa.

[0054] Example 2

[0055] A preparation method of an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway, comprising the following steps:

[0056] S1, according to the mass fraction, 100 parts of A type mixed monomer, 3 parts of B type composite catalyst, 1 part of B type catalytic promoter, 5 parts of reinforcing agent, 3 parts of antioxidant, 2 parts of flame retardant are added into the stirrer, heated to 22℃, stirred for 60 minutes, uniformly mixed, to obtain grouting material A; wherein the A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0057] S2, according to the mass fraction, 100 parts of B type mixed monomer, 3 parts of A type composite catalyst, 2 parts of A type catalytic promoter, 5 parts of reinforcing agent, 2 parts of antioxidant, 3 parts of flame retardant are added into the stirrer, heated to 22℃, stirred for 80 minutes, uniformly mixed, to obtain grouting material B, wherein the B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0058] When used, the grouting material A and the grouting material B are mixed according to 1:1.

[0059] The viscosity of the grouting material A is 6.2 mPas, the viscosity of the grouting material B is 5.7 mPas, the curing time of the mixed grouting material A and grouting material B is 74 s, and the compressive strength after curing is 46 MPa.

[0060] Example 3

[0061] A preparation method of an ultra-low viscosity grouting material suitable for a coal mine powdery difficult-to-penetrate coal roadway, comprising the following steps:

[0062] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 2 parts, antioxidant 2 parts, flame retardant 1 part, add to the stirrer, temperature rise to 20 DEG C, stirring 57 minutes, uniform mixing, get grouting material A material; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0063] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 1-3 parts, A type catalytic promoter 2 parts, reinforcing agent 3 parts, antioxidant 2 parts, flame retardant 2 parts, add to the stirrer, temperature rise to 20 DEG C, stirring 75 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0064] Use the grouting material A material and grouting material B material according to 1:1 mixing.

[0065] After detection, the viscosity of grouting material A material is 8.9 mPas, the viscosity of grouting material B material is 6.4 mPas, the curing time of grouting material A material, grouting material B material after mixing is 88 s, and the compressive strength after mixing and curing is 45 MPa.

[0066] Example 4

[0067] A kind of preparation method of super low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0068] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 2 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature rise to 20 DEG C, stirring 55 minutes, uniform mixing, get grouting material A material; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0069] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 2 parts, A type catalytic promoter 2 parts, reinforcing agent 3 parts, antioxidant 2 parts, flame retardant 2 parts, add to the stirrer, temperature to 20℃, stirring 75 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0070] In use, grouting material A material and grouting material B material are mixed according to 1:1.

[0071] After detection, the viscosity of grouting material A material is 9.1 mPas, the viscosity of grouting material B material is 7.1 mPas, the curing time of grouting material A material and grouting material B material after mixing is 92 s, and the compressive strength after mixing and curing is 42 MPa.

[0072] Example 5

[0073] A kind of preparation method of ultra-low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0074] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 4 parts, antioxidant 3 parts, flame retardant 1 part, add to the stirrer, temperature to 20℃, stirring 58 minutes, uniform mixing, get grouting material A material;Wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0075] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 3 parts, A type catalytic promoter 1 part, reinforcing agent 4 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature to 20℃, stirring 75 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0076] In use, grouting material A material and grouting material B material are mixed according to 1:1.

[0077] After detection, the viscosity of grouting material A material is 9.9 mPas, the viscosity of grouting material B material is 7.4 mPas, the curing time of grouting material A material and grouting material B material after mixing is 107 s, and the compressive strength after mixing and curing is 40 MPa.

[0078] Example 6

[0079] A preparation method of an ultra-low viscosity grouting material suitable for a roadway of a powdery and difficult-to-penetrate coal body in a coal mine, comprising the following steps:

[0080] S1, according to the mass fraction, A mixed monomer 100 parts, B composite catalyst 3 parts, B catalytic promoter 1 part, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 1 part are taken and added to the stirrer, heated to 18℃, stirred for 58 minutes, uniformly mixed to obtain grouting material A material; wherein the A mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0081] S2, according to the mass fraction, B mixed monomer 100 parts, A composite catalyst 1 part, A catalytic promoter 2 parts, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 3 parts are taken and added to the stirrer, heated to 22℃, stirred for 75 minutes, uniformly mixed to obtain grouting material B material, wherein the B mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0082] When used, the grouting material A material and the grouting material B material are mixed according to 0.8:1.

[0083] After detection, the viscosity of the grouting material A material is 7.2 mPas, the viscosity of the grouting material B material is 5.5 mPas, the curing time of the mixed grouting material A material and grouting material B material is 70s, and the compressive strength after mixing and curing is 42MPa.

[0084] Example 7

[0085] A preparation method of an ultra-low viscosity grouting material suitable for a roadway of a powdery and difficult-to-penetrate coal body in a coal mine, comprising the following steps:

[0086] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 3 parts, antioxidant 1 part, flame retardant 2 parts, add to the stirrer, temperature rise to 18 DEG C, stirring 60 minutes, uniform mixing, get grouting material A material; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0087] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 2 parts, A type catalytic promoter 1 part, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature rise to 20 DEG C, stirring 72 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0088] Use the grouting material A material and grouting material B material according to 1.2:1 mixing.

[0089] After detection, the viscosity of grouting material A material is 7.1 mPas, the viscosity of grouting material B material is 6 mPas, the curing time of grouting material A material, grouting material B material after mixing is 81 s, and the compressive strength after mixing and curing is 46 MPa.

[0090] Example 8

[0091] A kind of preparation method of super low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0092] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 4 parts, antioxidant 3 parts, flame retardant 1 part, add to the stirrer, temperature rise to 20 DEG C, stirring 55 minutes, uniform mixing, get grouting material A material;Wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0093] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 1 part, A type catalytic promoter 2 parts, reinforcing agent 4 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature rise to 18 DEG C, stirring 70 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, phenylalanine, pyrrole lysine and alanine mass ratio is 2:1:1.

[0094] When using, grouting material A material and grouting material B material are mixed according to 0.8:1.2.

[0095] After detection, the viscosity of grouting material A material is 9mPas, the viscosity of grouting material B material is 6.2mPas, the curing time of grouting material A material and grouting material B material after mixing is 87s, and the compressive strength after mixing and curing is 42MPa.

[0096] Example 9

[0097] A kind of preparation method of ultra-low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0098] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 2 parts, antioxidant 1 part, flame retardant 2 parts, add to the stirrer, temperature rise to 22 DEG C, stirring 60 minutes, uniform mixing, get grouting material A material;Wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid mass ratio is 1:1:2:1:7:2;

[0099] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 3 parts, A type catalytic promoter 2 parts, reinforcing agent 3 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature rise to 22 DEG C, stirring 70 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, phenylalanine, pyrrole lysine and alanine mass ratio is 2:1:1.

[0100] When using, grouting material A material and grouting material B material are mixed according to 1.2:0.8.

[0101] After detection, the viscosity of grouting material A material is 8.3mPas, the viscosity of grouting material B material is 5.6mPas, the curing time of grouting material A material and grouting material B material after mixing is 86s, and the compressive strength after mixing and curing is 47MPa.

[0102] Example 10

[0103] A preparation method of an ultra-low viscosity grouting material suitable for a roadway of a powdery and difficult-to-penetrate coal body in a coal mine, comprising the following steps:

[0104] S1, according to the mass fraction, A mixed monomer 100 parts, B composite catalyst 3 parts, B catalytic promoter 1 part, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 2 parts are added to the stirrer, heated to 18℃, stirred for 60 minutes, uniformly mixed, and grouting material A material is obtained; wherein the A mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, and the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0105] S2, according to the mass fraction, B mixed monomer 100 parts, A composite catalyst 1 part, A catalytic promoter 2 parts, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 2 parts are added to the stirrer, heated to 18℃, stirred for 80 minutes, uniformly mixed, and grouting material B material is obtained, wherein the B mixed monomer includes phenylalanine, pyrrole lysine and alanine, and the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0106] When in use, the grouting material A material and the grouting material B material are mixed according to 1:1.2.

[0107] After detection, the viscosity of the grouting material A material is 8.7mPas, the viscosity of the grouting material B material is 6.2mPas, the curing time of the mixed grouting material A material and grouting material B material is 77s, and the compressive strength after mixing and curing is 46MPa.

[0108] Example 11

[0109] A preparation method of an ultra-low viscosity grouting material suitable for a roadway of a powdery and difficult-to-penetrate coal body in a coal mine, comprising the following steps:

[0110] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 3 parts, antioxidant 3 parts, flame retardant 1 part, add to the stirrer, temperature rise to 22 DEG C, stirring 59 minutes, uniform mixing, get grouting material A material; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0111] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 2 parts, A type catalytic promoter 2 parts, reinforcing agent 2 parts, antioxidant 2 parts, flame retardant 1 part, add to the stirrer, temperature rise to 22 DEG C, stirring 73 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0112] Use the grouting material A material and grouting material B material according to 1.2:1 mixing.

[0113] After detection, the viscosity of grouting material A material is 8.8 mPas, the viscosity of grouting material B material is 5.9 mPas, the curing time of grouting material A material, grouting material B material after mixing is 76 s, and the compressive strength after mixing and curing is 45 MPa.

[0114] Example 12

[0115] A kind of preparation method of super low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0116] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 5 parts, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature rise to 22 DEG C, stirring 60 minutes, uniform mixing, get grouting material A material;Wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0117] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 2 parts, A type catalytic promoter 1 part, reinforcing agent 2 parts, antioxidant 2 parts, flame retardant 2 parts, add to the stirrer, temperature to 22 ℃, stirring 75 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0118] In use, the grouting material A material and the grouting material B material are mixed according to 1.1:1.

[0119] After detection, the viscosity of the grouting material A material is 7.8 mPas, the viscosity of the grouting material B material is 5.8 mPas, the curing time of the mixed grouting material A material and the grouting material B material is 76 s, and the compressive strength after mixing and curing is 45 MPa.

[0120] Comparative example 1

[0121] A kind of preparation method of ultra-low viscosity grouting material suitable for coal mine powdery difficult penetration coal roadway, comprising the following steps:

[0122] S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 1 part, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature to 35 ℃, stirring 55 minutes, uniform mixing, get grouting material A material;Wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexene diacid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:2;

[0123] S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 1 part, A type catalytic promoter 1 part, reinforcing agent 1 part, antioxidant 1 part, flame retardant 1 part, add to the stirrer, temperature to 35 ℃, stirring 70 minutes, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0124] In use, the grouting material A material and the grouting material B material are mixed according to 1:1.

[0125] After detection, the viscosity of the grouting material A material is 2.5 mPas, the viscosity of the grouting material B material is 2.9 mPas, the curing time of the mixed grouting material A material and the grouting material B material is 216 s, and the compressive strength after mixing and curing is 23 MPa.

[0126] Comparative Example 2

[0127] A preparation method of an ultra-low viscosity grouting material suitable for a roadway of a pulverous and difficult-to-penetrate coal body of a coal mine, comprising the following steps:

[0128] S1, according to the mass fraction, A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 1 part, antioxidant 1 part, flame retardant 1 part are taken and added to the stirrer, heated to 18 DEG C, stirred for 55 minutes, uniformly mixed, and A material of grouting material is obtained; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl ester acrylic acid is 1:1:2:1:7:8;

[0129] S2, according to the mass fraction, B type mixed monomer 100 parts, A type composite catalyst 1 part, A type catalytic promoter 1 part, reinforcing agent 1 part, antioxidant 1 part, flame retardant 1 part are taken and added to the stirrer, heated to 18 DEG C, stirred for 70 minutes, uniformly mixed, and B material of grouting material is obtained, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, and the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1.

[0130] When used, A material of grouting material and B material of grouting material are mixed according to 1:1.

[0131] After detection, the viscosity of A material of grouting material is 3.6 mPas, the viscosity of B material of grouting material is 5.3 mPas, the curing time of A material of grouting material and B material of grouting material after mixing is 186 s, and the compressive strength after mixing and curing is 25 MPa.

[0132] In the description of the present application, it should be understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0133] In addition, the terms "first", "second", etc. are used only to describe different instances, and are not used to indicate or imply relative importance or a number of indications of the technical features indicated. Therefore, the features defined as "first", "second" can explicitly or implicitly include at least one of the features. In the description of the present application, the meaning of "a plurality of" is at least two, such as two, three, etc., unless otherwise explicitly specified and limited.

[0134] In the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connecting", "connecting", "fixing" and the like should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or it can be integrated; it can be mechanically connected, or it can be electrically connected or in communication with each other; it can be directly connected, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise explicitly limited. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0135] In the present application, unless otherwise explicitly specified and limited, the first feature is "on" or "under" the second feature, which can be direct contact between the first and second features, or indirect contact between the first and second features through an intermediate medium. Moreover, the first feature "above", "above" and "above" the second feature can be directly above or obliquely above the first feature, or only indicate that the horizontal height of the first feature is higher than that of the second feature. The first feature "below", "below" and "below" the second feature can be directly below or obliquely below the first feature, or only indicate that the horizontal height of the first feature is less than that of the second feature.

[0136] In the present application, the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" mean that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In the present description, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples. Furthermore, those skilled in the art can combine and combine different embodiments or examples described in the present description and the features of different embodiments or examples without contradiction.

[0137] Although the embodiments of the present application have been shown and described above, it is understood that the above embodiments are exemplary and cannot be construed as limiting the present application, and those skilled in the art can make changes, modifications, replacements and variations to the above embodiments within the scope of the present application.

Claims

1. A method for preparing an ultra-low viscosity grouting material suitable for use in a roadway in a coal mine in a pulverous, low permeability coal body, characterized in that, It comprises the following steps: S1, according to the mass fraction of A type mixed monomer 100 parts, B type composite catalyst 3 parts, B type catalytic promoter 1 part, reinforcing agent 1-5 parts, antioxidant 1-3 parts, flame retardant 1-2 parts, heating stirring, uniform mixing, get grouting material A material; wherein, A type mixed monomer includes acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl acrylate, the mass ratio of acrylic acid, 3-butenoic acid, 2-hexenoic acid, 2-propyl heptyl acrylic acid, 2-acetylamino-3-phenyl acrylic acid and 2-hydroxyethyl acrylate is 1:1:2:1:7:2; S2, according to the mass fraction of B type mixed monomer 100 parts, A type composite catalyst 1-3 parts, A type catalytic promoter 1-2 parts, reinforcing agent 1-5 parts, antioxidant 1-2 parts, flame retardant 1-3 parts, heating stirring, uniform mixing, get grouting material B material, wherein B type mixed monomer includes phenylalanine, pyrrole lysine and alanine, the mass ratio of phenylalanine, pyrrole lysine and alanine is 2:1:1, the A type composite catalyst comprises cyclotriphosphazene base and 2-imidazolidone, the mass ratio of cyclotriphosphazene base and 2-imidazolidone is 1:1, the A type catalytic promoter comprises 2-methyl imidazole and benzimidazole, the mass ratio of 2-methyl imidazole and benzimidazole is 7:1; In the step S1, when heating stirring, the temperature is raised to 18-22℃, stirring for 55-60 minutes, the speed is 1500 revolutions / minute, in the step S2, when heating stirring, the temperature is raised to 18-22℃, stirring for 70-80 minutes; The grouting material A material and the grouting material B material are mixed in the ratio of (0.8-1.2):(0.8-1.2) when used; The B type composite catalyst comprises platinum black and palladium powder, the mass ratio of platinum black and palladium powder is 1:3; The B type catalytic promoter comprises copper bromide and magnesium oxide, the mass ratio of copper bromide and magnesium oxide is 2:

1.

2. The method for preparing the ultra-low viscosity grouting material suitable for the roadway of the pulverous and low permeable coal body of the coal mine according to claim 1, characterized in that, The reinforcing agent comprises nano calcium carbonate, nano titanium dioxide and nano cesium carbonate, the mass ratio of nano calcium carbonate, nano titanium dioxide and nano cesium carbonate is 1:9:

2.

3. The method for preparing the ultra-low viscosity grouting material suitable for the roadway of the powdery and low permeable coal body of the coal mine according to claim 1, characterized in that, The antioxidant comprises tert-butyl hydroquinone and glutathione, the mass ratio of tert-butyl hydroquinone and glutathione is 4:

1.

4. The method for preparing the ultra-low viscosity grouting material suitable for the roadway of the powdery and low permeable coal body of the coal mine according to claim 1, characterized in that, The flame retardant comprises tributyl phosphate, tris(2-ethylhexyl) phosphate and tris(2-chloroethyl) phosphate, the mass ratio of tributyl phosphate, tris(2-ethylhexyl) phosphate and tris(2-chloroethyl) phosphate is 3:1:

1.

5. A super low viscosity grouting material prepared by the method of any one of claims 1 to 4, characterized in that, It comprises grouting material A material and grouting material B material, A type mixed monomer in grouting material A material and A type composite catalyst, A type catalytic promoter in grouting material B material occur in situ polymerization reaction, B type mixed monomer in grouting material B material and B type composite catalyst, B type catalytic promoter in grouting material A material occur in situ polymerization reaction.

Images