A raw material grinding aid

Abstract

The present invention discloses a raw material grinding aid, comprising triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic liquid, and water. The cement grinding aid prepared by the method of the present invention has a good grinding effect on cement, can significantly increase the fineness of cement, and improve the strength of cement.

Description

Technical Field

[0001] The present invention relates to the technical field of cement processing, in particular to a raw material grinding aid. Background Art

[0002] Cement grinding is a link with high energy consumption in the cement production process. By optimizing the grinding process, such as installing a roller press to pre-crush and grind the clinker, the subsequent grinding energy consumption can be greatly reduced, thereby reducing the energy consumption of the entire grinding process. In addition, the addition of cement grinding aids during the grinding process can aid grinding and reduce the agglomeration of cement particles in the cement mill and conveying equipment, accelerating the flow of cement in the production system, thereby achieving the effect of energy conservation and emission reduction.

[0003] At present, most of the grinding aids widely used in the raw meal grinding process have relatively simple functions. They have good effects in improving the raw meal grinding efficiency and reducing the grinding energy consumption. However, there is still much room for improvement in improving the burnability of raw meal and reducing the coal consumption of clinker burning. Summary of the Invention

[0004] To this end, the present invention provides a raw material grinding aid, the components of which include triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The preparation method of the iridium-titanium composite oxide is as follows:

[0005] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution;

[0006] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, then adding ammonia water into the reactor, sealing the reactor after the addition is completed, rapidly heating to 180-200°C, and keeping the temperature for more than 10 hours; after the insulation is completed, air-cooling to room temperature, opening the reactor, separating the mixed solution into solid and liquid, washing the solid phase with deionized water, and drying;

[0007] (3) The dried solid phase is calcined in a muffle furnace at 400-450° C. for more than 1 hour to obtain the iridium-titanium composite oxide.

[0008] Furthermore, the preparation method of the anionic ionic liquid is: mixing 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in dichloromethane, stirring the mixed mixture at room temperature for more than 3 hours, then placing the mixture in an environment of 50±2°C to evaporate the dichloromethane, washing the residual phase with deionized water to remove chlorine, and then vacuum drying to obtain the anionic ionic liquid.

[0009] Furthermore, the iridium-titanium composite oxide is subjected to surface modification treatment, and the treatment method is:

[0010] Step 1, dispersing the iridium-titanium composite oxide in xylene to form a first suspension, heating the first suspension to a boiling state, condensing and refluxing, and then adding γ-aminopropyltrimethoxysilane to the first suspension. After the addition is completed, continue heating, boiling, condensing and refluxing for more than 8 hours, and then air cool to room temperature, separate the solid and liquid, wash the solid phase with ethanol, and dry it to obtain a solid phase A;

[0011] Step 2: Dispersing the solid phase A in deionized water to form a second suspension, adding polyethylene glycol to the second suspension, rapidly stirring for more than 1 hour after the addition is completed, adding an aqueous solution of polyvinyl alcohol to the second suspension, stirring again for more than 1 hour after the addition is completed, and then adding methanol to the second suspension under stirring, and continuing to stir for more than 10 minutes after the addition is completed;

[0012] Step 3: After stirring, separate the second suspension into solid and liquid, heat the solid phase to 220° C. in an argon atmosphere and keep it warm for more than 3 hours, and then air-cool to room temperature in an argon atmosphere after the insulation, to obtain the surface-modified iridium-titanium composite oxide.

[0013] Furthermore, the components of the raw material grinding aid are calculated by weight as follows: 20-30 parts of triisopropanolamine, 5-8 parts of iridium-titanium composite oxide, 10-16 parts of sodium carboxymethyl cellulose, 8-12 parts of anionic ionic liquid, and 60 parts of water.

[0014] Furthermore, in the ethanol solution of tetrabutyl titanate, the volume percentage of tetrabutyl titanate is 11% to 14%; in the ethanol solution of iridium trichloride, the mass percentage of iridium trichloride is 2% to 3%, and the mixed volume ratio of the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride is 1:1.

[0015] Furthermore, the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution.

[0016] Furthermore, the mass ratio of 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 2-3:5-9:100.

[0017] Furthermore, the solid-liquid ratio of the iridium-titanium composite oxide dispersed in xylene is solid / liquid = 1 to 3 g / 100 mL, and the mass ratio of the added mass of the γ-aminopropyltrimethoxysilane to the iridium-titanium composite oxide is γ-aminopropyltrimethoxysilane: iridium-titanium composite oxide = 5 to 8 g: 1 to 3 g.

[0018] Furthermore, the solid-liquid ratio of the solid phase A dispersed in deionized water to form a second suspension is solid / liquid = 3 to 4 g / 100 mL; the mass percentage of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 3% to 4%; the mass ratio of the added amount of polyethylene glycol, polyvinyl alcohol aqueous solution, and methanol to the solid phase A is polyethylene glycol: polyvinyl alcohol aqueous solution: methanol: solid phase A = 16 to 18 g: 800 to 1000 mL: 80 to 100 mL: 3 to 4 g.

[0019] The beneficial effects of the present invention are that the cement grinding aid prepared by the method of the present invention has a good grinding aid effect on cement, can significantly increase the fineness of cement, and improve the strength of cement. DETAILED DESCRIPTION

[0020] The present invention will be further described below with reference to the embodiments.

[0021] Example 1

[0022] A raw material grinding aid comprises triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 20 parts of triisopropanolamine, 5 parts of iridium-titanium composite oxide, 10 parts of sodium carboxymethyl cellulose, 8 parts of anionic ionic liquid and 60 parts of water.

[0023] Wherein, the preparation method of the iridium-titanium composite oxide is:

[0024] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 11%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 2%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0025] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0026] (3) The dried solid phase was calcined in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide.

[0027] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 2:5:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0028] Example 2

[0029] A raw material grinding aid comprises triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 24 parts of triisopropanolamine, 6 parts of iridium-titanium composite oxide, 12 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0030] Wherein, the preparation method of the iridium-titanium composite oxide is:

[0031] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 12%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 2%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0032] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0033] (3) The dried solid phase was calcined in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide.

[0034] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 2:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0035] Example 3

[0036] A raw material grinding aid comprises triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of iridium-titanium composite oxide, 14 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0037] Wherein, the preparation method of the iridium-titanium composite oxide is:

[0038] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 13%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0039] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0040] (3) The dried solid phase was calcined in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide.

[0041] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0042] Example 4

[0043] A raw material grinding aid comprises triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 30 parts of triisopropanolamine, 8 parts of iridium-titanium composite oxide, 16 parts of sodium carboxymethyl cellulose, 12 parts of anionic ionic liquid and 60 parts of water.

[0044] Wherein, the preparation method of the iridium-titanium composite oxide is:

[0045] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 14%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0046] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0047] (3) The dried solid phase was calcined in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide.

[0048] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:9:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0049] Comparative Example 1

[0050] A raw material grinding aid comprises triisopropanolamine, surface-modified iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of surface-modified iridium-titanium composite oxide, 14 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0051] Wherein, the preparation method of the surface-modified iridium-titanium composite oxide is:

[0052] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 13%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0053] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0054] (3) calcining the dried solid phase in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide;

[0055] (4) Surface modification treatment, the treatment method is:

[0056] Step 1, dispersing the iridium-titanium composite oxide in xylene to form a first suspension, wherein the solid-liquid ratio of the iridium-titanium composite oxide dispersed in xylene is solid / liquid = 2g / 100mL; heating the first suspension to a boiling state, condensing and refluxing, and then adding γ-aminopropyltrimethoxysilane to the first suspension, wherein the mass ratio of the added mass of γ-aminopropyltrimethoxysilane to the iridium-titanium composite oxide is γ-aminopropyltrimethoxysilane:iridium-titanium composite oxide = 5g:2g; after the addition is completed, continuing to heat, boil, condense and reflux for 8h, and then air cooling to room temperature, solid-liquid separation, washing the solid phase with ethanol, and drying to obtain solid phase A;

[0057] Step 2, dispersing the solid phase A in deionized water to form a second suspension, the solid-liquid ratio of the solid phase A dispersed in deionized water to form the second suspension is solid / liquid = 3g / 100mL; adding polyethylene glycol (PEG1000) to the second suspension, and rapidly stirring at 200r / min for 1h after the addition is completed, adding polyvinyl alcohol (average degree of polymerization 1750±50) aqueous solution to the second suspension after the addition is completed, stirring again at 200r / min for 1h after the addition is completed, and then adding methanol to the second suspension under stirring, and continuing to stir at 200r / min for 10min after the addition is completed; wherein the mass percentage of polyvinyl alcohol in the aqueous solution of polyvinyl alcohol is 3%; the mass ratio of the polyethylene glycol, the aqueous solution of polyvinyl alcohol, and the methanol added to the solid phase A is polyethylene glycol: polyvinyl alcohol aqueous solution: methanol: solid phase A = 16g:1000mL:100mL:3g;

[0058] Step 3: After stirring, separate the second suspension into solid and liquid, heat the solid phase to 220° C. in an argon atmosphere and keep it for 3 hours, and then air-cool to room temperature in an argon atmosphere after the end of the insulation to obtain the surface-modified iridium-titanium composite oxide.

[0059] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0060] Comparative Example 2

[0061] A raw material grinding aid comprises triisopropanolamine, surface-modified iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of surface-modified iridium-titanium composite oxide, 14 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0062] Wherein, the preparation method of the surface-modified iridium-titanium composite oxide is:

[0063] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 13%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0064] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0065] (3) calcining the dried solid phase in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide;

[0066] (4) Surface modification treatment, the treatment method is:

[0067] Step 1, dispersing the iridium-titanium composite oxide in xylene to form a first suspension, wherein the solid-liquid ratio of the iridium-titanium composite oxide dispersed in xylene is solid / liquid = 2 g / 100 mL; heating the first suspension to a boiling state, condensing and refluxing, and then adding γ-aminopropyltrimethoxysilane to the first suspension, wherein the mass ratio of the added mass of γ-aminopropyltrimethoxysilane to the iridium-titanium composite oxide is γ-aminopropyltrimethoxysilane: iridium-titanium composite oxide = 7 g: 2 g; after the addition is completed, continuing to heat, boil, condense and reflux for 8 hours, then air cooling to room temperature, solid-liquid separation, washing the solid phase with ethanol, and drying to obtain solid phase A;

[0068] Step 2, dispersing the solid phase A in deionized water to form a second suspension, the solid-liquid ratio of the solid phase A dispersed in deionized water to form the second suspension is solid / liquid = 3g / 100mL; adding polyethylene glycol (PEG1000) to the second suspension, and rapidly stirring at 200r / min for 1h after the addition is completed, adding polyvinyl alcohol (average degree of polymerization 1750±50) aqueous solution to the second suspension after the addition is completed, stirring again at 200r / min for 1h after the addition is completed, and then adding methanol to the second suspension under stirring, and continuing to stir at 200r / min for 10min after the addition is completed; wherein the mass percentage of polyvinyl alcohol in the aqueous solution of polyvinyl alcohol is 3%; the mass ratio of the polyethylene glycol, the aqueous solution of polyvinyl alcohol, and the methanol added to the solid phase A is polyethylene glycol: polyvinyl alcohol aqueous solution: methanol: solid phase A = 17g:1000mL:100mL:4g;

[0069] Step 3: After stirring, separate the second suspension into solid and liquid, heat the solid phase to 220° C. in an argon atmosphere and keep it for 3 hours, and then air-cool to room temperature in an argon atmosphere after the end of the insulation to obtain the surface-modified iridium-titanium composite oxide.

[0070] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0071] Comparative Example 3

[0072] A raw material grinding aid comprises triisopropanolamine, surface-modified iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of surface-modified iridium-titanium composite oxide, 14 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0073] Wherein, the preparation method of the surface-modified iridium-titanium composite oxide is:

[0074] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 13%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0075] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0076] (3) calcining the dried solid phase in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide;

[0077] (4) Surface modification treatment, the treatment method is:

[0078] Step 1, dispersing the iridium-titanium composite oxide in xylene to form a first suspension, wherein the solid-liquid ratio of the iridium-titanium composite oxide dispersed in xylene is solid / liquid = 2g / 100mL; heating the first suspension to a boiling state, condensing and refluxing, and then adding γ-aminopropyltrimethoxysilane to the first suspension, wherein the mass ratio of the added mass of γ-aminopropyltrimethoxysilane to the iridium-titanium composite oxide is γ-aminopropyltrimethoxysilane:iridium-titanium composite oxide = 8g:2g; after the addition is completed, continuing to heat, boil, condense and reflux for 8h, and then air cooling to room temperature, solid-liquid separation, washing the solid phase with ethanol, and drying to obtain solid phase A;

[0079] Step 2, dispersing the solid phase A in deionized water to form a second suspension, the solid-liquid ratio of the solid phase A dispersed in deionized water to form the second suspension is solid / liquid = 3g / 100mL; adding polyethylene glycol (PEG1000) to the second suspension, and rapidly stirring at 200r / min for 1h after the addition is completed, adding polyvinyl alcohol (average degree of polymerization 1750±50) aqueous solution to the second suspension after the addition is completed, stirring again at 200r / min for 1h after the addition is completed, and then adding methanol to the second suspension under stirring, and continuing to stir at 200r / min for 10min after the addition is completed; wherein the mass percentage of polyvinyl alcohol in the aqueous solution of polyvinyl alcohol is 3%; the mass ratio of the polyethylene glycol, the aqueous solution of polyvinyl alcohol, and the methanol added to the solid phase A is polyethylene glycol: polyvinyl alcohol aqueous solution: methanol: solid phase A = 18g:1000mL:100mL:4g;

[0080] Step 3: After stirring, separate the second suspension into solid and liquid, heat the solid phase to 220° C. in an argon atmosphere and keep it for 3 hours, and then air-cool to room temperature in an argon atmosphere after the end of the insulation to obtain the surface-modified iridium-titanium composite oxide.

[0081] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0082] Comparative Example 4

[0083] A raw material grinding aid comprises triisopropanolamine, titanium dioxide powder, sodium carboxymethyl cellulose, anionic ionic liquid and water, wherein the components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of titanium dioxide powder, 14 parts of sodium carboxymethyl cellulose, 10 parts of anionic ionic liquid and 60 parts of water.

[0084] The preparation method of the anionic ionic liquid is as follows: 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate are mixed in dichloromethane, wherein the mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in the dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 3:7:100; the mixed mixture is stirred at 60 r / min for 3 hours at room temperature, and then the mixture is placed in an environment of 50±2°C to evaporate the dichloromethane, the residual phase is washed with deionized water to remove chlorine, and then vacuum dried to obtain the anionic ionic liquid.

[0085] Comparative Example 5

[0086] A raw material grinding aid comprises triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose and water. The components are calculated by weight as follows: 27 parts of triisopropanolamine, 7 parts of iridium-titanium composite oxide, 14 parts of sodium carboxymethyl cellulose and 60 parts of water.

[0087] Wherein, the preparation method of the iridium-titanium composite oxide is:

[0088] (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; wherein the volume percentage of tetrabutyl titanate in the ethanol solution of tetrabutyl titanate is 13%; the mass percentage of iridium trichloride in the ethanol solution of iridium trichloride is 3%, and the volume ratio of the ethanol solution of tetrabutyl titanate to the ethanol solution of iridium trichloride is 1:1;

[0089] (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, and then adding ammonia water into the reactor, wherein the mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution; after the addition is completed, the reactor is closed, and the temperature is quickly raised to 190±5°C and kept warm for 10 hours; after the insulation is completed, the reactor is air-cooled to room temperature, the reactor is opened, the mixed solution is separated into solid and liquid, the solid phase is washed with deionized water, and dried;

[0090] (3) The dried solid phase was calcined in a muffle furnace at 420° C. for 1 h to obtain the iridium-titanium composite oxide.

[0091] Example 5

[0092] The grinding aid obtained by the method described in each of the above-mentioned embodiments and comparative examples is used in cement grinding, and performance test is carried out, and the grinding time is 30min. The proportioning of cement used in the test is all identical, and the cement mass proportioning is: clinker 70%, gypsum 5%, slag 11%, and fly ash 14%. The grinding aid doping amount of each test group is 0.06%. According to the method described in national standard GB / T17671-1999, the strength of cement mortar after each embodiment and comparative example grinding is tested, and the specific surface area of cement after each embodiment and comparative example grinding is measured by digital display Blaine air permeability specific surface area measuring instrument, and the result is as shown in Table 1.

[0093] Table 1

[0094] experimental group 28d clinker compressive strength (MPa) <![CDATA[Specific surface area (m 2 / kg) <!-- 7 -->]]> Example 1 56.9 503 Example 2 57.4 516 Example 3 57.6 521 Example 4 57.1 510 Comparative Example 1 66.7 569 Comparative Example 2 67.0 578 Comparative Example 3 66.9 574 Comparative Example 4 42.8 431 Comparative Example 5 43.4 445

[0095] As shown in Table 1, the cement grinding aid prepared by the method of the present invention has a good grinding effect on cement, significantly increasing the fineness of cement and improving the strength of cement. This may be due to the fact that the present invention can effectively prevent cement particle agglomeration and promote the destruction of particle structure during the grinding process, thereby achieving the purpose of fineness.

[0096] The technical solutions provided by the present invention are described in detail above. For those skilled in the art, according to the ideas of the embodiments of the present invention, there may be changes in the specific implementation methods and application scopes. In summary, the contents of this specification should not be understood as limiting the present invention.

Claims

1. A raw material grinding aid, characterized in that: The components include triisopropanolamine, iridium-titanium composite oxide, sodium carboxymethyl cellulose, anionic ionic liquid and water. The preparation method of the iridium-titanium composite oxide is as follows: (1) preparing an ethanol solution of tetrabutyl titanate and an ethanol solution of iridium trichloride, and mixing the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride to form a mixed solution; (2) placing the mixed solution in a sealed reactor, heating the reactor to 60±5°C, then adding ammonia water into the reactor, sealing the reactor after the addition is completed, rapidly heating to 180-200°C, and keeping the temperature for more than 10 hours; after the insulation is completed, air-cooling to room temperature, opening the reactor, separating the mixed solution into solid and liquid, washing the solid phase with deionized water, and drying; (3) calcining the dried solid phase in a muffle furnace at 400-450° C. for more than 1 hour to obtain the iridium-titanium composite oxide; The preparation method of the anionic ionic liquid comprises: mixing 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in dichloromethane, stirring the mixture at room temperature for more than 3 hours, then placing the mixture in an environment of 50±2° C. to evaporate the dichloromethane, washing the residual phase with deionized water to remove chlorine, and then vacuum drying to obtain the anionic ionic liquid.

2. A raw material grinding aid according to claim 1, characterized in that, The iridium-titanium composite oxide is subjected to surface modification treatment, and the treatment method is: Step 1, dispersing the iridium-titanium composite oxide in xylene to form a first suspension, heating the first suspension to a boiling state, condensing and refluxing, and then adding γ-aminopropyltrimethoxysilane to the first suspension. After the addition is completed, continue heating, boiling, condensing and refluxing for more than 8 hours, and then air cool to room temperature, separate the solid and liquid, wash the solid phase with ethanol, and dry it to obtain a solid phase A; Step 2: Dispersing the solid phase A in deionized water to form a second suspension, adding polyethylene glycol to the second suspension, rapidly stirring for more than 1 hour after the addition is completed, adding an aqueous solution of polyvinyl alcohol to the second suspension, stirring again for more than 1 hour after the addition is completed, and then adding methanol to the second suspension under stirring, and continuing to stir for more than 10 minutes after the addition is completed; Step 3: After stirring, separate the second suspension into solid and liquid, heat the solid phase to 220° C. in an argon atmosphere and keep it warm for more than 3 hours, and then air-cool to room temperature in an argon atmosphere after the insulation, to obtain the surface-modified iridium-titanium composite oxide.

3. A raw material grinding aid according to claim 2, characterized in that, The components of the raw material grinding aid are calculated by weight as follows: 20-30 parts of triisopropanolamine, 5-8 parts of iridium-titanium composite oxide, 10-16 parts of sodium carboxymethyl cellulose, 8-12 parts of anionic ionic liquid, and 60 parts of water.

4. A raw material grinding aid according to claim 2, characterized in that, In the ethanol solution of tetrabutyl titanate, the volume percentage of tetrabutyl titanate is 11% to 14%; in the ethanol solution of iridium trichloride, the mass percentage of iridium trichloride is 2% to 3%, and the mixed volume ratio of the ethanol solution of tetrabutyl titanate and the ethanol solution of iridium trichloride is 1:

1.

5. A raw material grinding aid according to claim 2, characterized in that, The mass percentage of the solute in the ammonia water is 25%, and the added volume of the ammonia water is 1 / 4 of the volume of the mixed solution.

6. A raw material grinding aid according to claim 2, characterized in that, The mass ratio of the 1-butyl-3-methylimidazole chloride and sodium dodecylsulfonate in dichloromethane is 1-butyl-3-methylimidazole chloride: sodium dodecylsulfonate: dichloromethane = 2-3:5-9:

100.

7. A raw material grinding aid according to claim 2, characterized in that: The solid-liquid ratio of the iridium-titanium composite oxide dispersed in xylene is solid / liquid = 1 to 3 g / 100 mL, and the mass ratio of the added mass of the γ-aminopropyltrimethoxysilane to the iridium-titanium composite oxide is γ-aminopropyltrimethoxysilane: iridium-titanium composite oxide = 5 to 8 g: 1 to 3 g.

8. A raw material grinding aid according to claim 2, characterized in that: The solid-liquid ratio of the solid phase A dispersed in deionized water to form a second suspension is solid / liquid = 3-4 g / 100 mL; the mass percentage of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 3%-4%; the mass ratio of the added amount of polyethylene glycol, polyvinyl alcohol aqueous solution, and methanol to the solid phase A is polyethylene glycol: polyvinyl alcohol aqueous solution: methanol: solid phase A = 16-18 g: 800-1000 mL: 80-100 mL: 3-4 g.