Cement grinding aid and preparation method thereof

Abstract

The invention relates to the technical field of cement, and discloses a cement grinding aid and a preparation method thereof. The cement grinding aid is obtained by adding the silicon-containing quaternary ammonium salt, the maleic anhydride-triethanolamine functional monomer, the nano silicon dioxide and the lignin into a stirrer for stirring. The silicon-containing quaternary ammonium salt can reduce the particle aggregation phenomenon caused by static electricity in the grinding process, and the grinding efficiency is improved by improving the fluidity and dispersity of the cement; wherein hydroxyl groups can be adsorbed on the surfaces of cement particles, and the particles are easier to grind by reducing the surface energy of the particles or causing position migration of surface layer crystal lattices and reducing the strength and hardness of the particles, so that the cement grinding efficiency is improved, and meanwhile, the energy consumption is reduced; alcohol amine functional groups in the maleic anhydride-triethanolamine functional monomer are polar groups and are adsorbed on the surfaces of cement particles, so that the surface energy of the particles is reduced, the aggregation phenomenon among the particles is reduced, and the particle size distribution is improved, thereby improving the grinding efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of cement grinding aids, in particular to a cement grinding aid and a preparation method thereof. Background Art

[0002] In cement production, how to reduce energy consumption in the cement grinding process has always been a matter of great concern. Cement grinding aid is a chemical aid that can reduce energy consumption, improve cement hourly output, cement strength, and fluidity. Existing grinding aids mainly include two categories: solid grinding aids and liquid grinding aids. However, its grinding aid efficiency is low and the synthesis cost of grinding aids is high. Therefore, how to avoid this phenomenon is the key to solving the problem. For example, patent CN103771753B discloses a cement grinding aid and a preparation method thereof. By replacing traditional raw material synthesis grinding aids with cheap industrial waste liquid and waste sugar residue, the cost of grinding aids is reduced and it is more environmentally friendly, but its grinding aid efficiency needs to be improved. Summary of the invention

[0003] 1. Technical issues to be resolved

[0004] In view of the deficiencies of the prior art, the present invention provides a cement grinding aid and a preparation method thereof, which have good grinding aid effect.

[0005] (II) Technical solution

[0006] To achieve the above purpose, the present invention provides the following technical scheme: a cement grinding aid, comprising the following components by weight: 7-12 parts by weight of silicon-containing quaternary ammonium salt, 5-8 parts by weight of maleic anhydride-triethanolamine functional monomer, 10-16 parts by weight of nano silicon dioxide, 12-18 parts by weight of lignin, and 22-38 parts by weight of water.

[0007] Preferably, the preparation method of the silicon-containing quaternary ammonium salt is:

[0008] (1) Add 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mix well, react at 72-90° C. for 7-15 hours, filter, wash and dry to obtain intermediate 1;

[0009] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, reacting at 65-80° C. for 6-10 h. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0010] (3) Add intermediate 1 and intermediate 2 to acetonitrile solvent, stir and dissolve, then add chloroplatinic acid catalyst, raise the temperature to 75-85° C., wash and dry after the reaction is completed to obtain a silicon-containing quaternary ammonium salt.

[0011] Preferably, the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde in (1) is 1:2.2-2.26.

[0012] Preferably, the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol in (2) is 1:1.14-1.18.

[0013] Preferably, the mass ratio of intermediate 1, intermediate 2 and chloroplatinic acid catalyst in (3) is 1:0.85-0.95:0.036-0.04.

[0014] Preferably, the preparation method of the maleic anhydride-triethanolamine functional monomer is: add maleic anhydride to a reactor, heat it to 60-70°C, and after the maleic anhydride is fully dissolved, slowly add triethanolamine thereto, the dropping time is 2.5-3h, and after the dropping is completed, continue to keep warm and react for 1.5-2.5h. After the reaction is completed, cool to room temperature, wash and dry to obtain the maleic anhydride-triethanolamine functional monomer.

[0015] Preferably, the mass ratio of maleic anhydride to triethanolamine is 1:1.05-1.12.

[0016] Preferably, the preparation method of the cement grinding aid is: adding silicon-containing quaternary ammonium salt, maleic anhydride-triethanolamine functional monomer, nano-silicon dioxide, and lignin into a stirrer, reacting at 75-90° C. for 35-45 minutes, and obtaining the cement grinding aid after the reaction is completed.

[0017] (III) Beneficial technical effects

[0018] The invention adds silicon-containing quaternary ammonium salt, maleic anhydride-triethanolamine functional monomer, nano silicon dioxide and lignin into a stirrer and stirs to obtain a cement grinding aid.

[0019] The amino group in 3,3-diaminobenzidine and the aldehyde group in p-hydroxybenzaldehyde were subjected to condensation reaction to introduce hydroxyl and alkenyl groups, thereby obtaining intermediate 1. The amino group and bromine group in hexamethyldisilazane and 3-bromo-1-propanol were subjected to quaternization reaction to generate quaternary ammonium salt groups and introduce hydroxyl groups to obtain intermediate 2. The alkenyl group in intermediate 1 and the silicon-hydrogen bond in intermediate 2 were subjected to addition reaction to obtain silicon-containing quaternary ammonium salt. Maleic anhydride and ethanolamine were subjected to ring-opening reaction to introduce ethanolamine functional groups, thereby obtaining maleic anhydride-triethanolamine functional monomers.

[0020] The cationic properties of silicon-containing quaternary ammonium salts can reduce the aggregation of particles caused by static electricity during the grinding process, and improve the grinding efficiency by improving the fluidity and dispersibility of cement; the hydroxyl groups therein can be adsorbed on the surface of cement particles, and reduce the strength and hardness of the particles by reducing the surface energy of the particles or causing the position migration of the surface layer crystal lattice, making the particles easier to be crushed, thereby improving the cement grinding efficiency and reducing energy consumption; the amine functional group in the maleic anhydride-triethanolamine functional monomer is a polar group, which is adsorbed on the surface of cement particles, reducing the surface energy of the particles, reducing the aggregation phenomenon between particles, and improving the particle size distribution, thereby improving the grinding efficiency. DETAILED DESCRIPTION

[0021] Example 1

[0022] (1) adding 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mixing evenly, wherein the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde is 1:2.2, reacting at 72° C. for 7 h, filtering, washing and drying after the reaction to obtain intermediate 1;

[0023] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, wherein the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol is 1:1.14, reacting at 65° C. for 6 h. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0024] (3) adding intermediate 1 and intermediate 2 to an acetonitrile solvent, stirring and dissolving, and then adding a chloroplatinic acid catalyst, wherein the mass ratio of intermediate 1, intermediate 2, and chloroplatinic acid catalyst is 1:0.85:0.036, heating to 75° C., washing and drying after the reaction is completed, to obtain a silicon-containing quaternary ammonium salt;

[0025] (4) adding maleic anhydride to the reactor, raising the temperature to 60° C., and after the maleic anhydride is fully dissolved, slowly adding triethanolamine dropwise thereto, wherein the mass ratio of maleic anhydride to triethanolamine is 1:1.05, and the dropping time is 2.5 hours. After the dropping is completed, the reaction is continued by keeping warm for 1.5 hours. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain a maleic anhydride-triethanolamine functional monomer;

[0026] (5) 7 parts by weight of silicon-containing quaternary ammonium salt, 5 parts by weight of maleic anhydride-triethanolamine functional monomer, 10 parts by weight of nano-silicon dioxide, 12 parts by weight of lignin, and 22 parts by weight of water are added into a stirrer, and reacted at 75° C. for 35 minutes. After the reaction is completed, a cement grinding aid is obtained.

[0027] Example 2

[0028] (1) adding 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mixing evenly, wherein the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde is 1:2.26, reacting at 90° C. for 15 h, filtering, washing and drying after the reaction to obtain intermediate 1;

[0029] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, wherein the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol is 1:1.18, reacting at 80° C. for 10 h. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0030] (3) adding intermediate 1 and intermediate 2 to an acetonitrile solvent, stirring and dissolving, and then adding a chloroplatinic acid catalyst, wherein the mass ratio of intermediate 1, intermediate 2, and chloroplatinic acid catalyst is 1:0.95:0.04, heating to 85° C., washing and drying after the reaction is completed, to obtain a silicon-containing quaternary ammonium salt;

[0031] (4) adding maleic anhydride to the reactor, raising the temperature to 70° C., and slowly dropping triethanolamine therein after the maleic anhydride is fully dissolved, wherein the mass ratio of maleic anhydride to triethanolamine is 1:1.12, and the dropping time is 3 h. After the dropping is completed, the reaction is continued by keeping the temperature for 2.5 h. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain a maleic anhydride-triethanolamine functional monomer;

[0032] (5) 12 parts by weight of silicon-containing quaternary ammonium salt, 8 parts by weight of maleic anhydride-triethanolamine functional monomer, 16 parts by weight of nano-silicon dioxide, 18 parts by weight of lignin, and 38 parts by weight of water are added into a stirrer, and reacted at 90° C. for 45 minutes. After the reaction is completed, a cement grinding aid is obtained.

[0033] Example 3

[0034] (1) Add 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mix well, wherein the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde is 1:2.24, react at 81° C. for 11 h, filter, wash and dry after the reaction to obtain intermediate 1;

[0035] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, wherein the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol is 1:1.16, reacting at 72.5°C for 8 hours. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0036] (3) adding intermediate 1 and intermediate 2 to an acetonitrile solvent, stirring and dissolving, and then adding a chloroplatinic acid catalyst, wherein the mass ratio of intermediate 1, intermediate 2, and chloroplatinic acid catalyst is 1:0.9:0.038, heating to 80° C., washing and drying after the reaction is completed, to obtain a silicon-containing quaternary ammonium salt;

[0037] (4) adding maleic anhydride to the reactor, raising the temperature to 65° C., and slowly dropping triethanolamine therein after the maleic anhydride is fully dissolved, wherein the mass ratio of maleic anhydride to triethanolamine is 1:1.08, and the dropping time is 2.7 h. After the dropping is completed, the reaction is continued at room temperature for 2 h. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain a maleic anhydride-triethanolamine functional monomer;

[0038] (5) 9.5 parts by weight of silicon-containing quaternary ammonium salt, 6.5 parts by weight of maleic anhydride-triethanolamine functional monomer, 13 parts by weight of nano-silicon dioxide, 15 parts by weight of lignin, and 30 parts by weight of water are added into a stirrer, and reacted at 82° C. for 40 minutes. After the reaction is completed, a cement grinding aid is obtained.

[0039] Example 4

[0040] (1) Add 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mix well, wherein the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde is 1:2.2, react at 72° C. for 7 h, filter, wash and dry after the reaction to obtain intermediate 1;

[0041] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, wherein the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol is 1:1.14, reacting at 65°C for 6 hours, and after the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0042] (3) adding intermediate 1 and intermediate 2 to an acetonitrile solvent, stirring and dissolving, and then adding a chloroplatinic acid catalyst, wherein the mass ratio of intermediate 1, intermediate 2, and chloroplatinic acid catalyst is 1:0.95:0.04, heating to 85° C., washing and drying after the reaction is completed, to obtain a silicon-containing quaternary ammonium salt;

[0043] (4) adding maleic anhydride to the reactor, raising the temperature to 70° C., and slowly dropping triethanolamine therein after the maleic anhydride is fully dissolved, wherein the mass ratio of maleic anhydride to triethanolamine is 1:1.12, and the dropping time is 3 h. After the dropping is completed, the reaction is continued by keeping the temperature for 2.5 h. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain a maleic anhydride-triethanolamine functional monomer;

[0044] (5) 9.5 parts by weight of silicon-containing quaternary ammonium salt, 6.5 parts by weight of maleic anhydride-triethanolamine functional monomer, 13 parts by weight of nano-silicon dioxide, 15 parts by weight of lignin, and 30 parts by weight of water are added into a stirrer, and reacted at 82° C. for 40 minutes. After the reaction is completed, a cement grinding aid is obtained.

[0045] Example 5

[0046] (1) Add 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mix well, wherein the mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde is 1:2.24, react at 81° C. for 11 h, filter, wash and dry after the reaction to obtain intermediate 1;

[0047] (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, wherein the mass ratio of hexamethyldisilazane to 3-bromo-1-propanol is 1:1.16, reacting at 72.5°C for 8 hours. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2;

[0048] (3) adding intermediate 1 and intermediate 2 to an acetonitrile solvent, stirring and dissolving, and then adding a chloroplatinic acid catalyst, wherein the mass ratio of intermediate 1, intermediate 2, and chloroplatinic acid catalyst is 1:0.85:0.036, heating to 75° C., washing and drying after the reaction is completed, to obtain a silicon-containing quaternary ammonium salt;

[0049] (4) adding maleic anhydride to the reactor, raising the temperature to 60° C., and after the maleic anhydride is fully dissolved, slowly adding triethanolamine dropwise thereto, wherein the mass ratio of maleic anhydride to triethanolamine is 1:1.05, and the dropping time is 2.5 hours. After the dropping is completed, the reaction is continued by keeping warm for 1.5 hours. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain a maleic anhydride-triethanolamine functional monomer;

[0050] (5) 12 parts by weight of silicon-containing quaternary ammonium salt, 8 parts by weight of maleic anhydride-triethanolamine functional monomer, 16 parts by weight of nano-silicon dioxide, 18 parts by weight of lignin, and 38 parts by weight of water are added into a stirrer, and reacted at 90° C. for 45 minutes. After the reaction is completed, a cement grinding aid is obtained.

[0051] Comparative Example 1

[0052] This comparative example is compared with Example 5, except that no silicon-containing quaternary ammonium salt is added.

[0053] The cement grinding aids of Examples 1-5 and Comparative Example 1 of the present invention were made into 20 wt % aqueous solutions, and 0.04 wt % of the aqueous solutions were evenly sprayed on the surface of the cement material to be ground. The cement was ground for 20 min and the specific surface area of ​​the cement was tested. The test results are shown in Table 1.

[0054] Table 1: Grinding aids tested.

[0055]

[0056] It can be seen from Table 1 that, compared with Comparative Example 1, the specific surface area of ​​cement particles in Examples 1-5 of the present invention is increased.

[0057] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A cement grinding aid, characterized in that: The invention comprises the following components by weight: 7-12 parts by weight of silicon-containing quaternary ammonium salt, 5-8 parts by weight of maleic anhydride-triethanolamine functional monomer, 10-16 parts by weight of nano silicon dioxide, 12-18 parts by weight of lignin and 22-38 parts by weight of water.

2. The cement grinding aid according to claim 1, characterized in that The preparation method of the silicon-containing quaternary ammonium salt is: (1) Add 3,3-diaminobenzidine and p-hydroxybenzaldehyde to N,N-dimethylformamide solvent, mix well, react at 72-90° C. for 7-15 hours, filter, wash and dry to obtain intermediate 1; (2) adding hexamethyldisilazane and 3-bromo-1-propanol to N,N-dimethylformamide solvent, reacting at 65-80° C. for 6-10 h. After the reaction is completed, distilling under reduced pressure, washing with petroleum ether, and drying to obtain intermediate 2; (3) Add intermediate 1 and intermediate 2 to acetonitrile solvent, stir and dissolve, then add chloroplatinic acid catalyst, raise the temperature to 75-85° C., wash and dry after the reaction is completed to obtain a silicon-containing quaternary ammonium salt.

3. The silicon-containing quaternary ammonium salt according to claim 2, characterized in that The mass ratio of 3,3-diaminobenzidine to p-hydroxybenzaldehyde in (1) is 1:2.2-2.

26.

4. The silicon-containing quaternary ammonium salt according to claim 2, characterized in that The mass ratio of hexamethyldisilazane to 3-bromo-1-propanol in (2) is 1:1.14-1.

18.

5. The silicon-containing quaternary ammonium salt according to claim 2, characterized in that The mass ratio of intermediate 1, intermediate 2 and chloroplatinic acid catalyst in (3) is 1:0.85-0.95:0.036-0.

04.

6. The cement grinding aid according to claim 1, characterized in that The preparation method of the maleic anhydride-triethanolamine functional monomer is as follows: maleic anhydride is added into a reactor, the temperature is raised to 60-70° C., after the maleic anhydride is fully dissolved, triethanolamine is slowly added dropwise thereto for 2.5-3 hours, and after the addition is completed, the reaction is continued by keeping the temperature for 1.5-2.5 hours. After the reaction is completed, the reaction is cooled to room temperature, washed and dried to obtain the maleic anhydride-triethanolamine functional monomer.

7. The maleic anhydride-triethanolamine functional monomer according to claim 6, characterized in that: The mass ratio of maleic anhydride to triethanolamine is 1:1.05-1.

12.

8. A method for preparing a cement grinding aid according to any one of claims 1 to 7, characterized in that: The preparation method of the cement grinding aid comprises the following steps: adding silicon-containing quaternary ammonium salt, maleic anhydride-triethanolamine functional monomer, nano silicon dioxide and lignin into a stirrer, reacting at 75-90° C. for 35-45 minutes, and obtaining the cement grinding aid after the reaction is completed.

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