CN117342821A - Magnetized graphene-nano silicate gel and preparation method thereof - Google Patents
Magnetized graphene-nano silicate gel and preparation method thereof Download PDFInfo
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001879 gelation Methods 0.000 title description 2
- 239000004567 concrete Substances 0.000 claims abstract description 55
- 238000003756 stirring Methods 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 31
- 239000000725 suspension Substances 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 19
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 14
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- 230000005415 magnetization Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 29
- 235000012241 calcium silicate Nutrition 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 9
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 claims description 6
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 235000019976 tricalcium silicate Nutrition 0.000 claims description 6
- 229910021534 tricalcium silicate Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000005204 segregation Methods 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 2
- -1 and after standing Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000378 calcium silicate Substances 0.000 description 23
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 23
- 239000000047 product Substances 0.000 description 12
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 9
- 239000000920 calcium hydroxide Substances 0.000 description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 9
- 238000006703 hydration reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000007863 gel particle Substances 0.000 description 4
- 229920002521 macromolecule Polymers 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000006259 organic additive Substances 0.000 description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 206010016807 Fluid retention Diseases 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical group CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a magnetized graphene-nano silicate gel and a preparation method thereof, wherein the mass ratio of each component is weighed, nano silicon oxide and superfine grinding clinker are put into a planetary mixer for mixing, deionized water is added for mixing the gel component slurry, and after standing, deionized water and orthosilicic acid are added while mixing the slurry to obtain an initial silicate gel; then stirring and dripping a dissolving agent at a constant speed to obtain dissolved silicate gel, adding a nanocellulose solution into the dissolved silicate gel, adding a silane coupling agent, stirring to obtain a nano silicate gel suspension, adding graphene for magnetization, standing, filtering water and drying to obtain magnetized graphene-nano silicate gel powder, and applying the magnetized graphene-nano silicate gel powder to concrete, so that the bending and compressive strength of early concrete can be improved, and the cohesiveness and segregation phenomenon of the concrete can be improved.
Description
Technical Field
The invention relates to the technical field of silicate gel, in particular to magnetized graphene-nano silicate gel.
Background
In the ready-mixed concrete industry, the shortage of the multiplexing type additive for improving the workability and early strength of concrete at the same time can only additionally refer to the organic additives such as early strength agents and viscosity modifiers according to the requirements of the two additives respectively, and the use of the organic additives is often limited by raw materials, when the raw materials of the concrete change, the ratio of the organic additives to the original concrete can be in an inadaptation condition, the workability is controlled by adjusting the additives, and the phenomena of on-site water adding of material-viscosity workers or segregation, slurry and bone separation of the concrete are easy to occur, so that the concrete is difficult to pump due to poor workability. Therefore, it is required to design a product that effectively improves both early strength and workability of concrete.
Disclosure of Invention
The invention aims to solve the technical problems that: the invention provides a nano silicate gel and a preparation method thereof, which are used for solving the problems of concrete cohesiveness and difficult preparation of early strength and greatly reducing the possibility of concrete segregation.
The technical scheme of the invention is as follows: the magnetized graphene-nano silicate gel comprises, by weight, 19-29 parts of nano silicon oxide, 74-116 parts of superfine grinding clinker, 26-32 parts of orthosilicic acid, 1200-1800 parts of deionized water, 0.3-0.5 part of a dissolving agent, 0.7-1.3 part of graphene, 11-25 parts of a silane coupling agent and 24-36 parts of nano cellulose.
Preferably, the nano silicon oxide is prepared by a sol-gel method, the particle size is between 20 and 60nm, the purity is 99%, and the dosage is 22 to 26 parts.
Preferably, the superfine grinding clinker comprises one or more of ground tricalcium silicate and ground dicalcium silicate, wherein the ground tricalcium silicate is obtained by grinding tricalcium silicate by a high-fine powder grinding machine, the fineness is between 8 and 15 mu m, and the purity is 99%; the dicalcium silicate is obtained by grinding dicalcium silicate by a high-fine powder grinder, the fineness is between 8 and 15 mu m, the purity is 99%, and the dosage is 84 to 106 parts.
Preferably, the orthosilicic acid is colorless transparent colloid, and has a chemical formula of H 4 SiO 4 The density is 2.62-2.65 mg/m 3 The dosage is 28-30 parts.
Preferably, the stripping agent is CuSO 4 、FeSO 4 、Na 2 SO 4 One or more of the following.
Preferably, the graphene is used in an amount of 0.9 to 1.1 parts.
Preferably, the silane coupling agent is gamma-aminopropyl triethoxysilane, and the dosage is 14-22 parts.
Preferably, the width of the nanocellulose is 20-50 nm, the length is 0.8-2 um, the purity is 99%, and the dosage is 29-31 parts.
The deionized water is pure water which does not contain ionic substances after being treated.
The preparation method of the magnetized graphene-nano silicate gel comprises the following steps:
step one: weighing the components according to the mass ratio, adding nano silicon oxide and superfine grinding clinker into a planetary mixer to stir for 15s, adding 20-25 parts of deionized water into the planetary mixer to stir for 150s to obtain gel component slurry, adding 575-780 parts of deionized water and orthosilicic acid while stirring the slurry after standing for 240s, stirring for more than 300s after finishing feeding to obtain initial silicate gel, and standing the initial silicate gel for 150min; in the process, the superfine grinding clinker is subjected to hydration reaction to generate calcium hydroxide and hydrated calcium silicate gel, nano silicon oxide and calcium hydroxide in the product of the nano silicon oxide can be subjected to secondary reaction to generate hydrated calcium silicate gel, so that the calcium silicate product is increased, part of calcium hydroxide can be consumed at the same time, and the concentration of the hydrated calcium silicate gel is increased; meanwhile, after the orthosilicic acid is added, residual calcium hydroxide can be consumed to form hydrated calcium silicate gel, and on the other hand, redundant orthosilicic acid is dissolved and then dispersed between clinker particles and hydrated calcium silicate products, and self-polycondensation reaction is carried out in deionized water medium to form the polycondensate silicic acid with a net-shaped structure, and the structure has stronger water retention performance, so that the surface tension of the hydrated calcium silicate gel suspension is improved, and a state with non-Newtonian fluid characteristics is formed. In order to prevent calcium silicate gel formed in the whole hydration reaction process from being overlapped with each other to form a continuous strength structural unit, more deionized water is added for continuous stirring to disperse the calcium silicate hydrate products, so that the single nano calcium silicate hydrate is formed. The condensed silicic acid in the suspension keeps the clinker which is not reacted and the hydrated calcium silicate in a dispersed state, so that the subsequent overlapping formation of a large particle structure of hydration reaction products is avoided.
Step two: stirring the initial silicate gel after standing at the speed of 300r/min, dripping a dissolving agent at a constant speed, controlling the dripping time to be 30-35 min to obtain a dissolved silicate gel, and simultaneously adding the nanocellulose into 600-1000 parts of deionized water to be stirred and dissolved to obtain a nanocellulose solution;
step three: adding a nano cellulose solution into dissolved silicate gel, stirring for 60s at a speed of 500r/min, then adding a silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding graphene into the suspension, uniformly stirring at a speed of 30r/min, magnetizing the suspension in a magnetic field of 900-1200G for 120min, standing the suspension for 24h after magnetization, filtering excessive water by a filter press, putting a filter-pressed product into an oven, setting the temperature of the oven at 60-80 ℃, and baking for 48h to obtain magnetized graphene-nano silicate gel powder.
In the second and third steps, the free calcium in the suspension is absorbed by the dissolving agent, so that the purity of the reaction product is further improved. In an aqueous medium, ethoxysilane groups of a silane coupling agent are hydrolyzed to form silanol, the surface of nano cellulose contains a large number of hydroxyl groups, the silanol and hydroxyl groups are subjected to condensation reaction to form stable covalent bonds, unreacted hydroxyl groups on the surface of the nano cellulose are adsorbed on the surface of hydrated calcium silicate gel, in addition, magnetized graphene is oxidized by the hydroxyl groups on the surface of the nano cellulose under the action of magnetic force to form oxidized graphene, the oxidized graphene is uniformly distributed to all corners of a suspension, and the magnetized graphene-nano silicate gel capable of adjusting concrete cohesiveness and early strength is obtained after the dried at a specific temperature.
Application of magnetized graphene-nano silicate gel in concrete.
The beneficial effects of the invention are as follows:
1. in addition to the hydrated calcium silicate, the superfine grinding clinker is also accompanied with the generation of a large amount of calcium hydroxide products in the hydration reaction process, and the addition of calcium hydroxide into concrete can damage the effect of the water reducing agent, so that the working performance loss of the concrete is increased, and most of redundant calcium hydroxide is consumed while the hydrated calcium silicate is generated through the reaction of nano silicon oxide and orthosilicate with the calcium hydroxide. And the sulfate is used as a stripping agent, so that the residual calcium hydroxide is further consumed to generate harmless calcium sulfate micro-solubles, and the purity of silicate gel in the suspension is improved;
2. the magnetized graphene-nano hydrated calcium silicate gel powder is mixed into concrete, and after the magnetized graphene-nano hydrated calcium silicate gel powder is fully stirred, the magnetized graphene-nano hydrated calcium silicate gel particles are uniformly dispersed into concrete slurry, silanol ends of a silane coupling agent and nano cellulose are adsorbed on the surface of the nano hydrated calcium silicate, and a large number of hydroxyl groups on the surface of the nano cellulose increase the hydrogen bonding acting force of water molecules, so that the concrete slurry becomes more viscous, the flow among the water molecules is reduced due to a reticular structure formed by condensation silicic acid attached to the periphery, and the cohesiveness of the whole fluid of the concrete is improved;
3. after the magnetized graphene-nano hydrated calcium silicate gel powder is mixed into concrete, nano calcium silicate gel particles uniformly dispersed into concrete slurry can fully exert an 'induction molding' effect, a strength structure formed by hydration of a gel material slurry in the concrete can be rapidly molded on the nano calcium silicate gel particles and are mutually connected to form strength, meanwhile, the components of the nano calcium silicate gel particles are the same as the hydration product components of the concrete gel material slurry, the nano calcium silicate gel can be well filled between gaps formed after the concrete is hardened, the generation of microcracks is reduced, the early strength of the concrete is effectively improved, and the possibility of cracking of the concrete is reduced;
4. along with the progress of hydration reaction of concrete slurry, the alkalinity in the concrete is improved, nano cellulose is not adsorbed on the surface of nano silicate gel any more, the nano cellulose in the concrete slurry is subjected to polycondensation reaction in an alkaline environment to form long-chain fiber macromolecules, and the fiber macromolecules are distributed in a strength structure of the hardened concrete; simultaneously, the magnetized graphene reacts under the action of hydroxyl and magnetic force to form graphene oxide, the dispersibility of the graphene oxide is far higher than that of the graphene oxide, and when the graphene oxide is in slurry of concrete, the magnetized graphene can be uniformly distributed in the concrete under the superposition of the dispersing action and the magnetic force action. The fiber macromolecules and the graphene are materials with high toughness and high tensile strength, and the toughness of the concrete can be greatly improved and the bending resistance of the concrete can be improved under the dual actions of the fiber macromolecules and the magnetized graphene.
Detailed Description
The technical solution of the present invention is further illustrated by the following detailed description, which is given by way of illustration and not limitation.
Example 1: the preparation of the magnetized graphene-nano silicate gel comprises the following steps:
(1) The weight portions are as follows: adding 19 parts of nano silicon oxide and 74 parts of superfine grinding clinker into a planetary mixer to stir for 15s, adding 20 parts of deionized water into the planetary mixer to stir for 150s to obtain gel component slurry, adding 580 parts of deionized water and 26 parts of orthosilicic acid while stirring the slurry after the slurry is kept stand for 240s, stirring for more than 300s after the feeding is finished to obtain initial silicate gel, and keeping the initial silicate gel stand for 150min.
(2) Stirring the initial silicate gel after standing in the step (1) at a speed of 300r/min, dropwise adding 0.4 part of dissolving agent at a constant speed, and controlling the dropwise adding time to be 30-35 min to obtain the dissolved silicate gel. Simultaneously, 24 parts of nano cellulose is put into 680 parts of deionized water to be stirred and dissolved, so as to obtain a nano cellulose solution.
(3) Adding the nano cellulose solution in the step (2) into the dissolved silicate gel, stirring for 60s at the speed of 500r/min, then adding 11 parts of silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding 0.7 part of graphene into the suspension, uniformly stirring at the speed of 30r/min, and magnetizing the suspension in a magnetic field of 900-1200G for 120min. After magnetization, standing the suspension for 24 hours, then press-filtering excessive water by using a press filter, putting a press-filtered product into a baking oven, setting the temperature of the baking oven at 60-80 ℃, and baking for 48 hours to obtain the magnetized graphene-nano silicate gel powder.
Example 2: the preparation of the magnetized graphene-nano silicate gel comprises the following steps:
(1) The weight portions are as follows: adding 22 parts of nano silicon oxide and 84 parts of superfine grinding clinker into a planetary mixer to mix for 15s, adding 22 parts of deionized water into the planetary mixer to mix for 150s to obtain gel component slurry, adding 640 parts of deionized water and 28 parts of orthosilicic acid while mixing the slurry after the slurry is kept stand for 240s, mixing for more than 300s after the material addition is finished to obtain initial silicate gel, and keeping the initial silicate gel stand for 150min.
(2) Stirring the initial silicate gel after standing in the step (1) at a speed of 300r/min, dropwise adding 0.4 part of dissolving agent at a constant speed, and controlling the dropwise adding time to be 30-35 min to obtain the dissolved silicate gel. Meanwhile, 29 parts of nanocellulose is put into 738 parts of deionized water to be stirred and dissolved, so that nanocellulose solution is obtained.
(3) Adding the nano cellulose solution in the step (2) into the dissolved silicate gel, stirring for 60s at the speed of 500r/min, then adding 14 parts of silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding 0.9 part of graphene into the suspension, uniformly stirring at the speed of 30r/min, and magnetizing the suspension in a magnetic field of 900-1200G for 120min. After magnetization, standing the suspension for 24 hours, then press-filtering excessive water by using a press filter, putting a press-filtered product into a baking oven, setting the temperature of the baking oven at 60-80 ℃, and baking for 48 hours to obtain the magnetized graphene-nano silicate gel powder.
Example 3: the preparation of the magnetized graphene-nano silicate gel comprises the following steps:
(1) The weight portions are as follows: adding 26 parts of nano silicon oxide and 106 parts of superfine grinding clinker into a planetary mixer to stir for 15s, adding 24 parts of deionized water into the planetary mixer to stir for 150s to obtain gel component slurry, adding 720 parts of deionized water and 30 parts of orthosilicic acid while stirring the slurry after the slurry is kept stand for 240s, stirring for more than 300s after the material addition is finished to obtain initial silicate gel, and keeping the initial silicate gel stand for 150min.
(2) Stirring the initial silicate gel after standing in the step (1) at a speed of 300r/min, dropwise adding 0.4 part of dissolving agent at a constant speed, and controlling the dropwise adding time to be 30-35 min to obtain the dissolved silicate gel. Simultaneously, 31 parts of nanocellulose is put into 856 parts of deionized water to be stirred and dissolved, so as to obtain nanocellulose solution.
(3) Adding the nano cellulose solution in the step (2) into the dissolved silicate gel, stirring for 60s at the speed of 500r/min, then adding 22 parts of silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding 1.1 parts of graphene into the suspension, uniformly stirring at the speed of 30r/min, and magnetizing the suspension in a magnetic field of 900-1200G for 120min. After magnetization, standing the suspension for 24 hours, then press-filtering excessive water by using a press filter, putting a press-filtered product into a baking oven, setting the temperature of the baking oven at 60-80 ℃, and baking for 48 hours to obtain the magnetized graphene-nano silicate gel powder.
Example 4: the preparation of the magnetized graphene-nano silicate gel comprises the following steps:
(1) The weight portions are as follows: 29 parts of nano silicon oxide and 116 parts of superfine grinding clinker are put into a planetary mixer to be mixed for 15s, 25 parts of deionized water is added into the planetary mixer to be mixed for 150s, gel component slurry is obtained, after the slurry is kept stand for 240s, 780 parts of deionized water and 32 parts of orthosilicic acid are added while the slurry is mixed, after the material is added, the mixture is mixed for more than 300s, initial silicate gel is obtained, and the initial silicate gel is kept stand for 150min.
(2) Stirring the initial silicate gel after standing in the step (1) at a speed of 300r/min, dropwise adding 0.4 part of dissolving agent at a constant speed, and controlling the dropwise adding time to be 30-35 min to obtain the dissolved silicate gel. Simultaneously, 36 parts of nanocellulose is put into 995 parts of deionized water to be stirred and dissolved, so as to obtain nanocellulose solution.
(3) Adding the nano cellulose solution in the step (2) into the dissolved silicate gel, stirring for 60s at the speed of 500r/min, then adding 25 parts of silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding 1.3 parts of graphene into the suspension, uniformly stirring at the speed of 30r/min, and magnetizing the suspension in a magnetic field of 900-1200G for 120min. After magnetization, standing the suspension for 24 hours, then press-filtering excessive water by using a press filter, putting a press-filtered product into a baking oven, setting the temperature of the baking oven at 60-80 ℃, and baking for 48 hours to obtain the magnetized graphene-nano silicate gel powder.
The magnetized graphene-nano silicate gel prepared in the examples 1-4 is respectively doped into C30 and C60 marked concrete according to the proportion of 5% of cementing materials, and the proportion of the concrete is shown in the following table according to the parts by weight:
TABLE 1 concrete mix ratio
Comparative example 1 was set up, with the difference from example 3 that the graphene addition and magnetization procedure was eliminated, and the remaining components and processes were the same.
In addition, a control group was set, control group 1 was C30 concrete without nano silicate gel, and control group 2 was C60 concrete without nano silicate gel. The properties are shown in tables 2 and 3, and the strength unit is MPa:
TABLE 2C30 concrete Performance index
Table 3C60 concrete Performance index
As can be seen from the results of tables 2 and 3, in both C30 and C60 grade concretes, the early strength (1 d and 7 d) of the concretes is greatly improved after the magnetized graphene-nano silicate gel is doped, for example, the 1d compressive strength fluctuation of the C30 and C60 concretes in example 3 is 345% and 169% respectively compared with the control group 1 and the control group 2. And the later strength is not lower than that of the control group under the condition that the early strength is greatly improved. And under the action of nanocellulose and magnetized graphene, the flexural strength of the concrete is greatly improved. In example 3, the 1d flexural strength rise of the C30 and C60 concrete reached 300% and 305%, respectively, as compared to control 1 and control 2.
In comparative example 1, in which the graphene and magnetization process were removed, the compressive strength of C30 at 7d and 28d was slightly improved, but the flexural strength at full age was reduced, and the flexural strength of C30 and C60 concrete 1d was reduced by 26% and 19%, respectively, as compared with example 3. The magnetized graphene-nano silicate gel obtained after the graphene and magnetization procedures are introduced can further improve the flexural strength of concrete.
After the magnetized graphene-nano silicate gel is doped, the cohesiveness and the water retention of the concrete are improved, so that the segregation resistance of the concrete is also greatly improved, and in examples 3-4, the segregation resistance of the C30 and C60 concrete is 99%.
Comprehensive comparison shows that when the formula value of the nano silicate gel is lower than the preferred range, the improvement effect and the workability on the early strength are not as good as those of the preferred range; above the preferred range, the strength of the concrete is not lower than the preferred range, but slump and expansion are rapidly decreased, and fluidity is far lower than the preferred range.
Comprehensive comparison shows that when the formula value of the nano silicate gel is lower than the preferred range, the improvement effect and the workability on the early strength are not as good as those of the preferred range; above the preferred range, the strength of the concrete is not lower than the preferred range, but slump and expansion are rapidly decreased, and fluidity is far lower than the preferred range.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (10)
1. The magnetized graphene-nano silicate gel is characterized by comprising, by weight, 19-29 parts of nano silicon oxide, 74-116 parts of superfine grinding clinker, 26-32 parts of orthosilicic acid, 1200-1800 parts of deionized water, 0.3-0.5 part of a stripping agent, 0.7-1.3 parts of graphene, 11-25 parts of a silane coupling agent and 24-36 parts of nano cellulose.
2. The nano silicate gel according to claim 1, wherein: the nano silicon oxide is prepared by a sol-gel method, the particle size is between 20 and 60nm, the purity is 99 percent, and the dosage is 22 to 26 parts.
3. The nano silicate gel according to claim 1, wherein: the superfine grinding clinker comprises one or more of ground tricalcium silicate and ground dicalcium silicate, wherein the ground tricalcium silicate is obtained by grinding tricalcium silicate by a high-fine powder grinding machine, the fineness is between 8 and 15 mu m, and the purity is 99%; the dicalcium silicate is obtained by grinding dicalcium silicate by a high-fine powder grinder, the fineness is between 8 and 15 mu m, the purity is 99%, and the dosage is 84 to 106 parts.
4. The nano silicate gel according to claim 1, wherein: the orthosilicic acid is colorless transparent colloid, and has a chemical formula of H 4 SiO 4 The density is 2.62-2.65 mg/m 3 The dosage is 28-30 parts.
5. The nano silicate gel according to claim 1, wherein: the stripping agent is CuSO 4 、FeSO 4 、Na 2 SO 4 One or more of the following.
6. The nano silicate gel according to claim 1, wherein: the dosage of the graphene is 0.9-1.1 parts.
7. The nano silicate gel according to claim 1, wherein: the silane coupling agent is gamma-aminopropyl triethoxysilane, and the dosage is 14-22 parts.
8. The nano silicate gel according to claim 1, wherein: the width of the nano cellulose is 20-50 nm, the length is 0.8-2 um, the purity is 99%, and the dosage is 29-31 parts.
9. A process for the preparation of nano silicate gel according to claims 1-8, characterized in that: the method comprises the following steps:
step one: weighing the components according to the mass ratio, adding nano silicon oxide and superfine grinding clinker into a planetary mixer to stir for 15s, adding 20-25 parts of deionized water into the planetary mixer to stir for 150s to obtain gel component slurry, adding 575-780 parts of deionized water and orthosilicic acid while stirring the slurry after standing for 240s, stirring for more than 300s after finishing feeding to obtain initial silicate gel, and standing the initial silicate gel for 150min;
step two: stirring the initial silicate gel after standing at the speed of 300r/min, dripping a dissolving agent at a constant speed, controlling the dripping time to be 30-35 min to obtain a dissolved silicate gel, and simultaneously adding the nanocellulose into 600-1000 parts of deionized water to be stirred and dissolved to obtain a nanocellulose solution;
step three: adding a nano cellulose solution into dissolved silicate gel, stirring for 60s at a speed of 500r/min, then adding a silane coupling agent into a stirrer, continuously stirring for 120s to obtain nano silicate gel suspension, adding graphene into the suspension, uniformly stirring at a speed of 30r/min, magnetizing the suspension in a magnetic field of 900-1200G for 120min, standing the suspension for 24h after magnetization, filtering excessive water by a filter press, putting a filter-pressed product into an oven, setting the temperature of the oven at 60-80 ℃, and baking for 48h to obtain magnetized graphene-nano silicate gel powder.
10. Use of a magnetized graphene-nanosilicate gel according to claims 1-9 in concrete.
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