CN112456846B - Multifunctional composite additive - Google Patents
Multifunctional composite additive Download PDFInfo
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- CN112456846B CN112456846B CN202011397247.3A CN202011397247A CN112456846B CN 112456846 B CN112456846 B CN 112456846B CN 202011397247 A CN202011397247 A CN 202011397247A CN 112456846 B CN112456846 B CN 112456846B
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- 239000000654 additive Substances 0.000 title claims abstract description 28
- 230000000996 additive effect Effects 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 92
- 235000013162 Cocos nucifera Nutrition 0.000 claims abstract description 54
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 54
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 38
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 38
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 21
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 claims abstract description 21
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 21
- 229940080314 sodium bentonite Drugs 0.000 claims abstract description 21
- 229910000280 sodium bentonite Inorganic materials 0.000 claims abstract description 21
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 21
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 21
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 21
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 21
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 21
- 239000010457 zeolite Substances 0.000 claims abstract description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 96
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 76
- 239000007790 solid phase Substances 0.000 claims description 75
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 68
- 239000007864 aqueous solution Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 238000002791 soaking Methods 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 36
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 27
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 18
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 18
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 16
- 238000012216 screening Methods 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims 3
- 239000004567 concrete Substances 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007605 air drying Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000004568 cement Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/325—Preparation by double decomposition
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a multifunctional composite additive, which comprises the raw materials of sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The composite admixture prepared by the invention has good optimization effect on concrete, and the application range of the concrete is expanded.
Description
Technical Field
The invention relates to the technical field of building material processing, in particular to a multifunctional composite additive.
Background
The existing concrete admixture is a product obtained by compounding according to the use requirement. The concrete admixture has a vital role in ensuring the workability and performance adjustment of concrete, is widely applied in various fields of large buildings at present, and becomes an indispensable material in concrete. At present, the development of concrete admixtures has experienced common water reducing agents, high-efficiency water reducing agents and the current third-generation high-performance water reducing agents, and under the large trend of national environmental protection and obsolete backward productivity, the quality of concrete is greatly reduced, the clinker mixing amount of cement is far lower than the national standard requirement, and the variety and mixing amount of additives are continuously increased. However, the quality of the concrete can not be reduced at the present stage, so that the concrete admixture is required to have better adaptability and optimization, and the sustainable development of the building construction industry is promoted.
Disclosure of Invention
Therefore, the invention provides a multifunctional composite additive, which comprises the raw materials of sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate.
Further, the raw materials are as follows by weight: 30-40 parts of sodium bentonite, 10-30 parts of silicon powder, 10-20 parts of zeolite powder, 7-16 parts of sodium sulfate, 10-20 parts of hydroxyapatite, 10-20 parts of coconut shell powder and 1-5 parts of sodium gluconate.
Further, the preparation method of the hydroxyapatite comprises the following steps:
1) preparing aqueous solutions of cerium nitrate and calcium nitrate, sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solutions of cerium nitrate and calcium nitrate to form a mixture, carrying out water bath on the mixture for more than 8 hours at the temperature of 60 +/-10 ℃, and carrying out air cooling to normal temperature after heat preservation;
2) and filtering the mixture, washing the solid phase with deionized water, drying, and calcining at 450-500 ℃ for 10-15 h to obtain the hydroxyapatite.
Further, in the aqueous solution of the cerium nitrate and the calcium nitrate, the concentration of the cerium nitrate is 0.02-0.05 mol/L, the concentration of the calcium nitrate is 0.1-0.2 mol/L, and the balance is water; the solid-to-liquid ratio of the added amount of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 1-2 g/100 mL; the ammonia content of the ammonia water is 25% by mass, and the amount of the added ammonia water is adjusted to the pH value of the mixture to be 10.5.
The preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting screened powder, adding the screened powder into hydrogen peroxide solution to form mixed solution, placing the mixed solution into a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 20-40 min, cooling to normal temperature after heat preservation, opening the container, filtering the mixed solution, and drying a solid phase to obtain a solid phase A;
step two, soaking the solid phase A in a silane coupling agent KH-550 at normal temperature for 30-40 min, taking out, drying at normal temperature, and baking at 130 +/-5 ℃ for 1-1.5 h to obtain a solid phase B;
and step three, soaking the solid phase B in a citric acid aqueous solution, soaking at the constant temperature of 65 +/-5 ℃ for 3-4 hours, filtering after soaking, washing the solid phase with deionized water, and drying to obtain the coconut shell powder.
Furthermore, the mass fraction of the solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10-20.
Further, the solid phase A is soaked in the silane coupling agent KH-550 at a solid-liquid mass ratio of 1: 8-10.
Further, in the aqueous solution of citric acid, the mass fraction of citric acid is 1% -3%, and the balance is water; the solid phase B is soaked in the citric acid aqueous solution, and the solid-liquid mass ratio of the solid phase B to the liquid phase B is 1: 8-10.
The invention has the beneficial effects that: tests prove that the composite admixture prepared by the invention is multifaceted in concrete optimization, has good effect and expands the application range of concrete.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A multifunctional composite additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 30 parts of sodium bentonite, 10 parts of silicon powder, 10 parts of zeolite powder, 7 parts of sodium sulfate, 10 parts of hydroxyapatite, 10 parts of coconut shell powder and 1 part of sodium gluconate. The multifunctional composite additive is obtained by uniformly mixing the raw materials according to the parts at normal temperature.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.02mol/L, the concentration of the calcium nitrate is 0.1mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 1g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 450 ℃ for 15 hours to obtain the hydroxyapatite.
The preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 20min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 8. Soaking at normal temperature for 30min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 1%, and the balance is water; the solid phase B is soaked in the citric acid aqueous solution, and the solid-liquid mass ratio of the solid phase B to the liquid phase B is 1: 8. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Example 2
A multifunctional composite additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 34 parts of sodium bentonite, 20 parts of silicon powder, 14 parts of zeolite powder, 10 parts of sodium sulfate, 13 parts of hydroxyapatite, 14 parts of coconut shell powder and 3 parts of sodium gluconate. The multifunctional composite additive is obtained by uniformly mixing the raw materials according to the parts at normal temperature.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.03mol/L, the concentration of the calcium nitrate is 0.1mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 1g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 460 ℃ for 13 hours to obtain the hydroxyapatite.
The preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 30min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 9. Soaking at normal temperature for 30min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 2%, and the balance is water; the solid phase B is immersed in an aqueous solution of citric acid at a solid-liquid mass ratio of 1: 9. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Example 3
A multifunctional composite additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 36 parts of sodium bentonite, 20 parts of silicon powder, 17 parts of zeolite powder, 13 parts of sodium sulfate, 17 parts of hydroxyapatite, 16 parts of coconut shell powder and 4 parts of sodium gluconate. The multifunctional composite additive is obtained by uniformly mixing the raw materials according to the parts at normal temperature.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.04mol/L, the concentration of the calcium nitrate is 0.2mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 2g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 480 ℃ for 12 hours to obtain the hydroxyapatite.
The preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 30min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 9. Soaking at normal temperature for 30min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 2%, and the balance is water; the solid phase B is immersed in an aqueous solution of citric acid at a solid-liquid mass ratio of 1: 9. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Example 4
A multifunctional composite additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 40 parts of sodium bentonite, 30 parts of silicon powder, 20 parts of zeolite powder, 16 parts of sodium sulfate, 20 parts of hydroxyapatite, 20 parts of coconut shell powder and 5 parts of sodium gluconate. The multifunctional composite additive is obtained by uniformly mixing the raw materials according to the parts at normal temperature.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.05mol/L, the concentration of the calcium nitrate is 0.2mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 2g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 500 ℃ for 10 hours to obtain the hydroxyapatite.
The preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 40min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 10. Soaking at normal temperature for 40min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 3%, and the balance is water; the solid phase B is immersed in an aqueous solution of citric acid at a solid-liquid mass ratio of 1: 10. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Comparative example 1
An additive comprises sodium bentonite, silicon powder, zeolite powder, sodium sulfate, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 40 parts of sodium bentonite, 30 parts of silicon powder, 20 parts of zeolite powder, 16 parts of sodium sulfate, 20 parts of coconut shell powder and 5 parts of sodium gluconate. The raw materials are uniformly mixed according to the parts at normal temperature to obtain the additive.
The preparation method of the coconut shell powder material in the comparative example comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 40min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 10. Soaking at normal temperature for 40min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 3%, and the balance is water; the solid phase B is immersed in an aqueous solution of citric acid at a solid-liquid mass ratio of 1: 10. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Comparative example 2
An additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 40 parts of sodium bentonite, 30 parts of silicon powder, 20 parts of zeolite powder, 16 parts of sodium sulfate, 20 parts of hydroxyapatite, 20 parts of coconut shell powder and 5 parts of sodium gluconate. The raw materials are uniformly mixed according to the parts at normal temperature to obtain the additive.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of calcium nitrate, wherein the concentration of the calcium nitrate is 0.2mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the added ammonium dihydrogen phosphate to the aqueous solution of the calcium nitrate is 2g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 500 ℃ for 10 hours to obtain the hydroxyapatite of the comparative example.
The preparation method of the coconut shell powder material in the comparative example comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting and screening the screened powder, and adding the powder into a hydrogen peroxide solution to form a mixed solution, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of the coconut shell powder added into the hydrogen peroxide solution is 1: 10. Placing the mixed solution in a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 40min, air-cooling to normal temperature after heat preservation is finished, opening the container, filtering the mixed solution, and drying the solid phase at 80 +/-5 ℃ to obtain a solid phase A;
and step two, soaking the solid phase A in a silane coupling agent KH-550, wherein the solid-liquid mass ratio of the solid phase A soaked in the silane coupling agent KH-550 is 1: 10. Soaking at normal temperature for 40min, taking out, air drying at normal temperature, and baking at 130 + -5 deg.C for 1h to obtain solid phase B;
step three, soaking the solid phase B in an aqueous solution of citric acid, wherein the mass fraction of the citric acid in the aqueous solution of the citric acid is 3%, and the balance is water; the solid phase B is immersed in an aqueous solution of citric acid at a solid-liquid mass ratio of 1: 10. Soaking at the constant temperature of 65 +/-5 ℃ for 3 hours, filtering after soaking, washing a solid phase with deionized water for 3 times, and drying at the temperature of 80 +/-5 ℃ to obtain the coconut shell powder.
Comparative example 3
An additive comprises sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite and sodium gluconate. The raw materials are as follows by weight: 40 parts of sodium bentonite, 30 parts of silicon powder, 20 parts of zeolite powder, 16 parts of sodium sulfate, 20 parts of hydroxyapatite and 5 parts of sodium gluconate. The raw materials are uniformly mixed according to the parts at normal temperature to obtain the additive of the comparative example.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.05mol/L, the concentration of the calcium nitrate is 0.2mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 2g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 500 ℃ for 10 hours to obtain the hydroxyapatite.
Comparative example 4
An additive is prepared from sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate. The raw materials are as follows by weight: 40 parts of sodium bentonite, 30 parts of silicon powder, 20 parts of zeolite powder, 16 parts of sodium sulfate, 20 parts of hydroxyapatite, 20 parts of coconut shell powder and 5 parts of sodium gluconate. The raw materials are uniformly mixed according to the parts at normal temperature to obtain the additive of the comparative example.
The preparation method of the hydroxyapatite comprises the following steps:
1) preparing an aqueous solution of cerium nitrate and calcium nitrate, wherein the concentration of the cerium nitrate is 0.05mol/L, the concentration of the calcium nitrate is 0.2mol/L, and the balance is water; sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solution of the cerium nitrate and the calcium nitrate to form a mixture, wherein the solid-to-liquid ratio of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 2g/100 mL; the ammonia content of the ammonia water is 25 percent by mass, and the amount of the added ammonia water is to adjust the pH value of the mixture to 10.5; the mixture is subjected to heat preservation for 8 hours at the temperature of 60 +/-10 ℃ in water bath, and air cooling is carried out to normal temperature after the heat preservation is finished;
2) and filtering the mixture, washing the solid phase with deionized water for 3 times, drying at 80 +/-5 ℃, and calcining at 500 ℃ for 10 hours to obtain the hydroxyapatite.
The coconut shell powder material of the comparative example is obtained by screening coconut shell powder through a 500-mesh screen and collecting the screened powder.
Example 5
The admixture prepared in the examples 1-4 and the comparative examples 1-4 is added into concrete, wherein the weight ratio of the concrete is 357g of common 42.5# cement, 1550g of standard sand and 255g of water, and the amount of the admixture is 7% of the mass of the concrete. Concrete without additives was used as a control. The compression strength of various samples is tested according to standard JTG E30-2005 'test regulations for road engineering cement and cement concrete', and the sulfate corrosion resistance test of various samples is tested according to national standard GB/T50082-2009 'test method for long-term performance and durability of common concrete', with the results shown in Table 1. As can be seen from Table 1, the composite admixture prepared by the invention can obviously improve the compressive strength and the sulfate corrosion resistance of concrete, so that the application range of the concrete is widened. Comparing example 4 with the comparative example, it can be seen that the hydroxyapatite prepared by the invention has an accelerating effect on the improvement of the concrete strength and has a small influence on the corrosion resistance, while the coconut shell powder has a large influence on the corrosion resistance and has strict requirements on the treatment method.
TABLE 1
The technical solutions provided by the present invention are described in detail above, and for those skilled in the art, the ideas according to the embodiments of the present invention may be changed in the specific implementation manners and the application ranges, and in summary, the content of the present description should not be construed as limiting the present invention.
Claims (7)
1. A multifunctional composite additive is characterized in that the raw materials comprise sodium bentonite, silicon powder, zeolite powder, sodium sulfate, hydroxyapatite, coconut shell powder and sodium gluconate; the raw materials are as follows by weight: 30-40 parts of sodium bentonite, 10-30 parts of silicon powder, 10-20 parts of zeolite powder, 7-16 parts of sodium sulfate, 10-20 parts of hydroxyapatite, 10-20 parts of coconut shell powder and 1-5 parts of sodium gluconate.
2. The multifunctional composite additive according to claim 1, wherein the preparation method of the hydroxyapatite comprises the following steps:
1) preparing aqueous solutions of cerium nitrate and calcium nitrate, sequentially adding ammonium dihydrogen phosphate and ammonia water into the aqueous solutions of cerium nitrate and calcium nitrate to form a mixture, carrying out water bath on the mixture for more than 8 hours at the temperature of 60 +/-10 ℃, and carrying out air cooling to normal temperature after heat preservation;
2) and filtering the mixture, washing the solid phase with deionized water, drying, and calcining at 450-500 ℃ for 10-15 h to obtain the hydroxyapatite.
3. The multifunctional composite additive according to claim 2, wherein in the aqueous solution of cerium nitrate and calcium nitrate, the concentration of cerium nitrate is 0.02-0.05 mol/L, the concentration of calcium nitrate is 0.1-0.2 mol/L, and the balance is water; the solid-to-liquid ratio of the added amount of the ammonium dihydrogen phosphate to the aqueous solution of the cerium nitrate and the calcium nitrate is 1-2 g/100 mL; the ammonia content of the ammonia water is 25% by mass, and the amount of the added ammonia water is adjusted to the pH value of the mixture to be 10.5.
4. The multifunctional composite additive of claim 1, wherein the preparation method of the coconut shell powder comprises the following steps:
step one, screening coconut shell powder through a 500-mesh screen, collecting screened powder, adding the screened powder into hydrogen peroxide solution to form mixed solution, placing the mixed solution into a closed container, sealing the container, heating to 160 +/-5 ℃, preserving heat for 20-40 min, cooling to normal temperature after heat preservation, opening the container, filtering the mixed solution, and drying a solid phase to obtain a solid phase A;
step two, soaking the solid phase A in a silane coupling agent KH-550 at normal temperature for 30-40 min, taking out, drying at normal temperature, and baking at 130 +/-5 ℃ for 1-1.5 h to obtain a solid phase B;
and step three, soaking the solid phase B in a citric acid aqueous solution, soaking at the constant temperature of 65 +/-5 ℃ for 3-4 hours, filtering after soaking, washing the solid phase with deionized water, and drying to obtain the coconut shell powder.
5. The multifunctional composite admixture according to claim 4, wherein the mass fraction of solute in the hydrogen peroxide solution is 30%, and the solid-liquid mass ratio of coconut shell powder added into the hydrogen peroxide solution is solid/liquid =1: 10-20.
6. The multifunctional composite additive according to claim 4, wherein the solid phase A is soaked in the silane coupling agent KH-550 at a solid-liquid mass ratio of solid to liquid =1: 8-10.
7. The multifunctional composite admixture according to claim 4, wherein in the citric acid aqueous solution, the mass fraction of citric acid is 1-3%, and the balance is water; the solid phase B is soaked in the citric acid aqueous solution, and the solid-liquid mass ratio of solid to liquid =1: 8-10.
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