A flame retardant inorganic quick-setting material and preparation method thereof

Abstract

A flame retardant inorganic quick-setting material and a preparation method thereof, which are prepared from the following raw materials: sulphoaluminate cement, aluminum-magnesium hydrotalcite, phosphorus slag powder, waste PBO fiber, quick-setting agent, water reducer, functional additive, 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additive comprises a structural unit introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid. The material has high strength, remarkable quick-setting and flame retardant effects, and is safe and environmentally friendly to use.

Description

Technical Field

[0001] The invention relates to the technical field of quick-setting materials, and in particular to a flame-retardant inorganic quick-setting material and a preparation method thereof. Background Art

[0002] my country is rich in coal resources. Coal is the main energy source in my country and occupies a dominant position in the energy structure. The healthy, stable and sustainable development of the coal industry is a major issue related to national energy security. At present, inorganic quick-setting materials are increasingly used in coal-rock reinforcement, filling and sealing, water and air leakage blocking in coal mines. However, inorganic quick-setting materials on the market have more or less problems such as insufficient strength and poor flame retardant effect.

[0003] In order to solve the above problems, researchers in the industry have done a lot of work. For example, the Chinese invention patent with the authorization announcement number CN104446274B discloses a high-strength quick-setting material, which includes sulphoaluminate cement, fly ash, silica fume, water reducer, underwater anti-dispersant, quick-setting agent and water; the weight ratio of sulphoaluminate cement: fly ash: silica fume is 26:1:1; the water reducer is polycarboxylic acid, and the amount is 0.2-0.3 parts by weight; the underwater anti-dispersant is hydroxyethyl cellulose, and the amount is 0.3-0.35 parts by weight; the quick-setting agent is a compound of formula I, and the amount is 0.05-0.2 parts by weight; the amount of water is 14-16 parts by weight. The quick-setting material of the present invention can greatly shorten the setting time. However, its flame retardancy and environmental protection performance still need to be further improved.

[0004] It can be seen that the development of a flame-retardant inorganic quick-setting material and its preparation method which has high strength, significant quick-setting and flame-retardant effects, is safe and environmentally friendly, meets market demand, has broad market value and application prospects, and is of great significance to promoting the development of the field of inorganic quick-setting materials. Summary of the invention

[0005] In view of this, the object of the present invention is to provide a flame retardant inorganic quick-setting material and a preparation method thereof which has high strength, significant quick-setting and flame retardant effects, and is safe and environmentally friendly.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] A flame retardant inorganic quick-setting material, made from the following raw materials in parts by weight: 10-20 parts of sulphoaluminate cement, 3-10 parts of aluminum-magnesium hydrotalcite, 3-5 parts of phosphorus slag powder, 1-3 parts of waste PBO fiber, 1-3 parts of quick-setting agent, 0.5-1 parts of water reducer, 0.8-2 parts of functional additives, and 0.3-0.5 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additives include the following monomers introduced Structural units: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid.

[0008] Preferably, the sulphoaluminate cement is fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa.

[0009] Preferably, the fineness of the aluminum-magnesium hydrotalcite is 100-400 mesh.

[0010] Preferably, the particle size of the phosphorus slag powder is 300-800 mesh.

[0011] Preferably, the waste PBO fiber is waste PBO fiber.

[0012] Preferably, the accelerating setting agent is at least one of bauxite, KRS-2 accelerating setting agent and AX-1 accelerating setting agent.

[0013] Preferably, the water reducing agent is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0014] Preferably, the preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, and an initiator to a high boiling point solvent, stirring and reacting at 60-70° C. in an inert gas atmosphere for 4-6 hours, and removing the solvent by rotary evaporation after the reaction is completed. Then, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialyzing it in water for 24-32 hours, then taking the supernatant in the dialysis bag, and removing water by rotary evaporation to obtain a functional additive.

[0015] Preferably, the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent is (1-3):1:0.3:0.1:1:(0.03-0.06):(15-25).

[0016] Preferably, the initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N,N-dimethylformamide, and N-methylpyrrolidone; and the inert gas is any one of nitrogen, helium, neon, and argon.

[0017] Another object of the present invention is to provide a method for preparing the flame retardant inorganic quick-setting material, comprising the following steps: mixing the raw materials uniformly by weight, adding them into water and continuing to stir them uniformly, controlling the water-cement ratio to (0.5-0.75):1, and obtaining the flame retardant inorganic quick-setting material.

[0018] The beneficial effects of adopting the above technical solution are:

[0019] (1) The method for preparing the flame-retardant inorganic quick-setting material provided by the present invention has simple process, convenient operation and control, low dependence on equipment, small capital investment, low energy consumption, high preparation efficiency and finished product qualification rate, is suitable for industrial production, and has high promotion and application value.

[0020] (2) The flame retardant inorganic quick-setting material provided by the present invention is made of the following raw materials in parts by weight: 10-20 parts of sulphoaluminate cement, 3-10 parts of aluminum-magnesium hydrotalcite, 3-5 parts of phosphorus slag powder, 1-3 parts of waste PBO fiber, 1-3 parts of accelerating agent, 0.5-1 parts of water reducing agent, 0.8-2 parts of functional additives, and 0.3-0.5 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; through the mutual cooperation and joint action of the raw materials, the manufactured product has high strength, remarkable quick-setting and flame retardant effects, and is safe and environmentally friendly to use.

[0021] (3) The flame-retardant inorganic quick-setting material provided by the present invention, the functional additive includes the structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid. The molecular structure of the functional additive contains structures such as amphoteric organic ion salt, phenylphosphine oxide, triazone, phenoxazine, epoxy group and carboxyl group. These structures, under the multiple effects of electronic effect, steric effect and conjugation effect, enable the functional additive to effectively improve the quick-setting effect, water-reducing effect and flame-retardant effect of the quick-setting material, and give the product excellent mechanical strength.

[0022] (4) The flame retardant inorganic quick-setting material provided by the present invention, the sulphoaluminate cement, aluminum-magnesium hydrotalcite, phosphorus slag powder and waste PBO fiber cooperate to effectively reduce the amount of cement used, improve the density of the internal structure of the material, and improve the mechanical strength and sealing performance; the raw materials do not contain halogen, and the environmental protection performance is better. DETAILED DESCRIPTION

[0023] In order to make the technical solution of the present invention better understood by the technical personnel in the field, and to make the above-mentioned features, purposes and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with the embodiments. The embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0024] The average diameter of the waste PBO fibers in the embodiments of the present invention is 3 μm and the length is 5 mm.

[0025] Example 1

[0026] A flame retardant inorganic quick-setting material is prepared from the following raw materials in parts by weight: 10 parts of sulphoaluminate cement, 3 parts of aluminum-magnesium hydrotalcite, 3 parts of phosphorus slag powder, 1 part of waste PBO fiber, 1 part of quick-setting agent, 0.5 parts of water reducer, 0.8 parts of functional additives, and 0.3 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additives include structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

[0027] The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 100 mesh; the particle size of the phosphorus slag powder is 300 mesh; the waste PBO fiber is waste PBO fiber; the quick-setting agent is bauxite; the water reducing agent is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0028] The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator to a high boiling point solvent, stirring and reacting at 60°C for 4 hours in an inert gas atmosphere, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 24 hours, and then The supernatant in the dialysis bag was taken, and the water was removed by rotary evaporation to obtain a functional additive; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent was 1:1:0.3:0.1:1:0.03:15; the initiator was azobisisobutyronitrile; the high boiling point solvent was dimethyl sulfoxide; and the inert gas was nitrogen. Through GPC testing, the number average molecular weight of the functional additive was 17350 g / mol, M W / M n =1.367; calculated by elemental analysis and weight change, the mass ratio of the structural units introduced by 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid is 0.99:1:0.28:0.1:0.98;

[0029] A method for preparing the flame retardant inorganic quick-setting material comprises the following steps: after mixing the raw materials uniformly by weight, adding them into water and continuing to stir them uniformly, controlling the water-cement ratio to 0.75:1, and obtaining the flame retardant inorganic quick-setting material.

[0030] Example 2

[0031] A flame retardant inorganic quick-setting material is prepared from the following raw materials in parts by weight: 13 parts of sulphoaluminate cement, 5 parts of aluminum-magnesium hydrotalcite, 3.5 parts of phosphorus slag powder, 1.5 parts of waste PBO fiber, 1.5 parts of accelerating setting agent, 0.6 parts of water reducing agent, 1.2 parts of functional additives, and 0.35 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additives include structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

[0032] The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 200 mesh; the particle size of the phosphorus slag powder is 400 mesh; the waste PBO fiber is waste PBO fiber; the accelerating setting agent is KRS-2 accelerating setting agent; the water reducing agent is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0033] The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator to a high boiling point solvent, stirring and reacting at 63°C for 4.5 hours in an inert gas atmosphere, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 26 hours, and then taking the dialysate. The supernatant in the bag is subjected to rotary evaporation to remove water to obtain a functional additive; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent is 1.5:1:0.3:0.1:1:0.04:17; the initiator is azobisisobutyronitrile; the high boiling point solvent is N,N-dimethylformamide; and the inert gas is helium.

[0034] A method for preparing the flame retardant inorganic quick-setting material comprises the following steps: mixing the raw materials uniformly by weight, adding them into water and stirring them uniformly, controlling the water-cement ratio to 0.7:1, and obtaining the flame retardant inorganic quick-setting material.

[0035] Example 3

[0036] A flame retardant inorganic quick-setting material is prepared from the following raw materials in parts by weight: 15 parts of sulphoaluminate cement, 6 parts of aluminum-magnesium hydrotalcite, 4 parts of phosphorus slag powder, 2 parts of waste PBO fiber, 2 parts of accelerating agent, 0.8 parts of water reducer, 1.3 parts of functional additive, and 0.4 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additive comprises a structural unit introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

[0037] The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 250 mesh; the particle size of the phosphorus slag powder is 500 mesh; the waste PBO fiber is waste PBO fiber; the quick-setting agent is AX-1 type quick-setting agent; the water reducing agent is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0038] The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator to a high boiling point solvent, stirring and reacting at 65°C for 5 hours in an inert gas atmosphere, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 28 hours, and then taking the dialysis bag. The supernatant in the precipitate bag is evaporated and water is removed by rotary evaporation to obtain a functional additive; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator and high boiling point solvent is 2:1:0.3:0.1:1:0.045:20; the initiator is azobisisobutyronitrile; the high boiling point solvent is N-methylpyrrolidine; and the inert gas is neon.

[0039] A method for preparing the flame retardant inorganic quick-setting material comprises the following steps: mixing the raw materials uniformly by weight, adding them into water and stirring them uniformly, controlling the water-cement ratio to 0.65:1, and obtaining the flame retardant inorganic quick-setting material.

[0040] Example 4

[0041] A flame retardant inorganic quick-setting material is prepared from the following raw materials in parts by weight: 18 parts of sulphoaluminate cement, 8 parts of aluminum-magnesium hydrotalcite, 4.5 parts of phosphorus slag powder, 2.5 parts of waste PBO fiber, 2.5 parts of accelerating setting agent, 0.9 part of water reducing agent, 1.8 parts of functional additive, and 0.45 part of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additive comprises a structural unit introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

[0042] The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 350 mesh; the particle size of the phosphorus slag powder is 700 mesh; the waste PBO fiber is waste PBO fiber; the accelerator is a mixture of bauxite, KRS-2 accelerator, and AX-1 accelerator in a mass ratio of 1:2:3; the water reducer is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0043] The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator to a high boiling point solvent, stirring and reacting at 68°C in an inert gas atmosphere for 5.5 hours, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 30 hours, then taking the supernatant in the dialysis bag, and removing water by rotary evaporation to obtain Functional additives; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent is 2.5:1:0.3:0.1:1:0.055:23; the initiator is azobisisobutyronitrile; the high boiling point solvent is a mixture of dimethyl sulfoxide, N,N-dimethylformamide, and N-methylpyrrolidone in a mass ratio of 1:2:3; the inert gas is argon.

[0044] A method for preparing the flame retardant inorganic quick-setting material comprises the following steps: mixing the raw materials uniformly by weight, adding them into water and stirring them uniformly, controlling the water-cement ratio to 0.6:1, and obtaining the flame retardant inorganic quick-setting material.

[0045] Example 5

[0046] A flame retardant inorganic quick-setting material is prepared from the following raw materials in parts by weight: 20 parts of sulphoaluminate cement, 10 parts of aluminum-magnesium hydrotalcite, 5 parts of phosphorus slag powder, 3 parts of waste PBO fiber, 3 parts of accelerating agent, 1 part of water reducing agent, 2 parts of functional additives, and 0.5 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additives include structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

[0047] The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 400 mesh; the particle size of the phosphorus slag powder is 800 mesh; the waste PBO fiber is waste PBO fiber; the accelerating agent is bauxite; the water reducing agent is A series of polycarboxylic acid high-performance water reducers provided by Jiangsu Subote New Materials Co., Ltd.

[0048] The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator to a high boiling point solvent, stirring and reacting at 70°C for 6 hours in an inert gas atmosphere, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 32 hours, and then The supernatant in the dialysis bag is taken, and water is removed by rotary evaporation to obtain a functional additive; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent is 3:1:0.3:0.1:1:0.06:25; the initiator is azobisisobutyronitrile; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is nitrogen.

[0049] A method for preparing the flame retardant inorganic quick-setting material comprises the following steps: mixing the raw materials uniformly according to weight, adding them into water and stirring them uniformly, controlling the water-cement ratio to 0.5:1, and obtaining the flame retardant inorganic quick-setting material.

[0050] Comparative Example 1

[0051] A flame retardant inorganic quick-setting material and a preparation method thereof, which are substantially the same as those of Example 1, except that phosphorus slag powder and 3,3'-diamino-4,4'-difluorodiphenyl sulfone are not added.

[0052] Comparative Example 2

[0053] A flame retardant inorganic quick-setting material and a preparation method thereof, which are substantially the same as those in Example 1, except that no functional additives and waste PBO fibers are added.

[0054] The flame retardant inorganic quick-setting materials described in Examples 1-5 and Comparative Examples 1-2 were subjected to performance tests. The test results are shown in Table 1. The test methods refer to the current national standards and conventional methods in the industry. The flame retardancy is measured by the flame burning time in the alcohol burner combustion experiment. The smaller the value, the better the flame retardancy.

[0055] Table 1

[0056]

[0057] It can be seen from Table 1 that the flame retardant inorganic quick-setting material disclosed in the embodiment of the present invention has better compressive strength, quick-setting performance and flame retardancy than the comparative example; the combined use of phosphorus slag powder, 3,3'-diamino-4,4'-difluorodiphenyl sulfone, functional additives and waste PBO fibers is beneficial to improving the above properties.

[0058] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions only describe the principles of the present invention. The present invention may be subject to various changes and improvements without departing from the spirit and scope of the present invention. These changes and improvements fall within the scope of the present invention. The scope of protection claimed by the present invention is defined by the attached claims and their equivalents.

Claims

1. A flame retardant inorganic quick-setting material, characterized in that: The invention is prepared from the following raw materials in parts by weight: 10-20 parts of sulphoaluminate cement, 3-10 parts of aluminum-magnesium hydrotalcite, 3-5 parts of phosphorus slag powder, 1-3 parts of waste PBO fiber, 1-3 parts of accelerating agent, 0.5-1 parts of water reducing agent, 0.8-2 parts of functional additives, and 0.3-0.5 parts of 3,3'-diamino-4,4'-difluorodiphenyl sulfone; the functional additives include structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl (4-vinylphenyl) phosphine oxide, 1,3-bis (oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6 (1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, and itaconic acid.

2. The flame retardant inorganic quick-setting material according to claim 1, characterized in that: The sulphoaluminate cement is a fast-hardening sulphoaluminate cement, and its 3-day strength is 42.5 MPa; the fineness of the aluminum-magnesium hydrotalcite is 100-400 meshes.

3. The flame retardant inorganic quick-setting material according to claim 1, characterized in that: The particle size of the phosphorus slag powder is 300-800 mesh; the waste PBO fiber is waste PBO fiber.

4. The flame retardant inorganic quick-setting material according to claim 1, characterized in that: The accelerating setting agent is at least one of bauxite, KRS-2 accelerating setting agent and AX-1 accelerating setting agent; the water reducing agent is Series of polycarboxylic acid high performance water reducing agents.

5. The flame retardant inorganic quick-setting material according to claim 1, characterized in that: The preparation method of the functional additive comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid and an initiator into a high boiling point solvent, stirring and reacting at 60-70°C for 4-6 hours in an inert gas atmosphere, removing the solvent by rotary evaporation after the reaction is completed, dissolving the crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in water for 24-32 hours, then taking the supernatant in the dialysis bag, and removing water by rotary evaporation to obtain the functional additive.

6. The flame retardant inorganic quick-setting material according to claim 5, characterized in that: The mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, diphenyl(4-vinylphenyl)phosphine oxide, 1,3-bis(oxiranylmethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 10-(4-vinylphenyl)-10H-phenoxazine, itaconic acid, initiator, and high boiling point solvent is (1-3):1:0.3:0.1:1:(0.03-0.06):(15-25).

7. The flame retardant inorganic quick-setting material according to claim 5, characterized in that: The initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N,N-dimethylformamide, and N-methylpyrrolidone; and the inert gas is any one of nitrogen, helium, neon, and argon.

8. A method for preparing the flame retardant inorganic quick-setting material according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: mixing the raw materials uniformly according to weight, adding the raw materials into water and stirring the mixture uniformly, controlling the water-cement ratio to be (0.5-0.75):1, and obtaining a flame retardant inorganic quick-setting material.

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