CN108249806A - A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete - Google Patents
A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete Download PDFInfo
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- CN108249806A CN108249806A CN201711331837.4A CN201711331837A CN108249806A CN 108249806 A CN108249806 A CN 108249806A CN 201711331837 A CN201711331837 A CN 201711331837A CN 108249806 A CN108249806 A CN 108249806A
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- 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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- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention relates to a kind of preparation method of hydrated calcium silicate early strength agent and using the non-evaporating foster C30 self-compacting concretes prepared by the early strength agent；It is effectively utilized the discarded rice husk of acid processing and produces the waste liquid of calcium lignosulfonate as raw material, not only energy conservation and environmental protection, also reduce the production cost of hydrated calcium silicate early strength agent；And, the hydrated calcium silicate early strength agent prepared using the waste liquid that acid handles discarded rice husk and produces calcium lignosulfonate is with using the silicon sources such as sodium metasilicate and the hydrated calcium silicate early strength agent similar nature prepared using calcium sources such as calcium nitrate, can effectively improve the early strength and later strength of cement-based material.
Description
Technical field
Preparation method and use the present invention relates to building material field more particularly to a kind of hydrated calcium silicate early strength agent should
The self-compacting concrete of early strength agent.
Background technology
In the production process of precast concrete, to accelerate the turn-around speed of mold, improving production efficiency, frequently with
The mode of steam curing and addition early strength agent improves the early strength of concrete, when shortening the form removal of precast concrete with this
Between.And primary product of the hydrated calcium silicate as hydrated cementitious, early strength agent is used as, forming core position can be provided for hydrated cementitious
Point reduces energy when hydrated product is precipitated and hinders, promotes the progress of crystallization reaction, so as to improve hydrated cementitious speed, to carry
The early strength of high cement-based material.
At present, the preparation method of hydrated calcium silicate mainly has hydro-thermal method and chemical coprecipitation.Hydro-thermal method prepares aquation silicon
During sour calcium, temperature-pressure is needed, high energy consumption during production, and hydrated calcium silicate grain size obtained is larger, specific surface area is smaller, it is unfavorable
In the early strength for improving hydrated calcium silicate；And chemical coprecipitation has the advantages that simple for process, low energy consumption, can avoid height
The working environment of warm high pressure, but when preparing hydrated calcium silicate using chemical coprecipitation, silicon source used is the silicon salt such as sodium metasilicate,
Calcium source used increases hydrated calcium silicate for calcium salts, these silicon salt calcium salt higher prices such as calcium nitrate, calcium acetate or calcium chloride
Production cost.
Rich in silicon salt in the rice husk discarded after grain harvest, silicon salt therein acid can be dissolved out, as preparation aquation silicon
The silicon source of sour calcium；And produce in the waste liquid of calcium lignosulfonate rich in calcium ion, it may be used as preparing the calcium source of hydrated calcium silicate.
Using the waste liquid for producing calcium lignosulfonate as calcium source, discarded rice husk is handled as silicon source by sour, rice husk is not only solved and gives up
The Utilizing question of liquid also reduces the production cost of hydrated calcium silicate early strength agent.And the hydrated calcium silicate that the method is prepared is early strong
Agent can improve the early strength of cement-based material, can also improve the later strength of cement-based material, and be conducive to improve cement
The durability of sill.
Invention content
The technical problem to be solved by the present invention is to：At present, the preparation method of hydrated calcium silicate mainly has hydro-thermal method and chemistry
Coprecipitation, hydro-thermal method need temperature-pressure, and energy consumption is high, and are unfavorable for improving the early strong effect of hydrated calcium silicate；And change
Silicon source used in coprecipitation is learned as the silicon salt such as sodium metasilicate, calcium source is the calcium salts such as calcium nitrate, calcium acetate or calcium chloride, these silicon salt and
Calcium salt higher price increases the production cost of hydrated calcium silicate；Lack less energy consumption in the prior art and can make profits again simultaneously
The method that hydrated calcium silicate early strength agent is prepared with waste material.
The technical solution adopted by the present invention to solve the technical problems is：A kind of preparation side of hydrated calcium silicate early strength agent
Method, it is characterised in that：This method includes the following steps：
（1）Obtain silicon source；
（2）Obtain calcium source；
（3）Calcium source and silicon source are mixed in ultra-pure water, gel dispersal agent is added in and polyacrylamide is uniformly dispersed, keep pH value of solution
Value is more than 12, and constant temperature multi-step mixing filters drying, hydrated calcium silicate early strength agent is obtained after screening after complete reaction.
Further, step（1）Middle acquisition silicon source includes the following steps：
（1.1）Rice husk is selected to clean rice husk repeatedly with distilled water 3 ~ 5 times as silicon source；
（1.2）Step will be passed through（1.1）Rice husk after cleaning impregnates 12 ~ 48 h in 0.5 ~ 1mol/L hydrochloric acid solutions, with steaming
Distilled water cleans rice husk repeatedly until solution filters out after being in neutrality；
（1.3）Step will be passed through（1.2）Rice husk after cleaning is placed in 100 DEG C of air dry oven dry 24 h；
（1.4）The rice husk of above-mentioned acidizing pretreatment is placed in chamber type electric resistance furnace, with 10 DEG C/min heating rates from room temperature
It is taken out after to 400 ~ 800 DEG C of 1 h of roasting, grinding obtains white rice hull ash；
（1.5）It is 1 in mass ratio by 0.5 ~ 1mol/L NaOH solutions and rice hull ash：2 ~ 3 input retort, it is anti-at 40 ~ 80 DEG C
Answer 0.5 ~ 2h, after reaction, obtain silicon source after vacuum filtration.
Further, step（2）Middle acquisition calcium source includes the following steps：
The waste liquid of production calcium lignosulfonate is selected as calcium source.
Further, step（3）Described in the preparation method of ultra-pure water be：
Deionized water is boiled into 10 ~ 30min of heating, and nitrogen is passed through into water during heating, obtains ultra-pure water, it will
The ultra-pure water prepared is detected using CO-2 analyser, and the concentration of carbon dioxide in water is made to be less than 100ppm.
Further, step（3）Described in the preparation method of gel dispersal agent be：
Using the cetyl trimethylammonium bromide of cationic surfactant（CTAB）With the inorganic salts six with cyclic structure
Sodium metaphosphate（SHMP）Compounding is used as gel dispersal agent, wherein, the additive amount ratio of CTAB and SHMP are 4:6, using light splitting light
The absorbance of solution under degree measurement examination different situations judges the dispersion effect of solution with this.
Further, step（3）Middle multi-step mixing step is：60 DEG C are heated to using temperature control magnetic stirring apparatus, is carried out permanent
Warm multi-step mixing；
0 ~ 2h of phase keeps magnetic stirring apparatus rotating speed reaction raw materials to be made to be sufficiently mixed uniformly in 200 ~ 300rpm before the reaction；
2 ~ 10h of phase holding magnetic stirring apparatus rotating speeds improve reaction rate in 800 ~ 1000rpm, holding higher rotation speed in the reaction,
React fully completion；
10 ~ 12h of phase keeps magnetic stirring apparatus rotating speed in 200 ~ 300rpm after the reaction so that reaction product is dispersed in water-soluble
In liquid.
Further, step（3）It is middle to filter dry step and be：
Solution after above-mentioned constant temperature stepwise reaction is filtered, after suction filtration, filter residue is poured into beaker, and filtrate carries out
Secondary suction filtration washs filter residue with ultra-pure water repeatedly, removes undesired impurities and the complete sample of unreacted, filter residue is placed in 40 DEG C
It is dried in vacuum drying chamber to constant weight, is put into and has kept dry in CaO drying vessel.
Further, step（3）Middle screening step is：Sample sifter is selected as precentagewise：Grain size is less than the sample of 50nm
Gross sample 5 ~ 10% is accounted for, 50 ~ 200nm accounts for 80 ~ 85%, and surplus is more than 200nm.
Further, the present invention also provides it is a kind of be added with using the above method prepare hydrated calcium silicate early strength agent from
Hydrated calcium silicate early strength agent is applied to C30 self-compacting concretes by air-free concrete, wherein：1m3250Kg is included in concrete
Portland cement 42.5,75Kg flyash, 750Kg sand, 290Kg handstones, the big stones of 760Kg, 150Kg water, quality are mixed
Measure the polypropylene fibre for 0.1%, 25.2g cellulose ethers, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and cementitious material mass percent
For 10 ~ 15% nucleus type early strength agent.
Further, the preparation method of self-compacting concrete is：
Using forced mixer, wet-mixing after first dry mixing first adds in big stone, handstone and sand, starts forced mixer, stirs
Mix 40 ~ 60s；Portland cement 42.5 and flyash are added, starts forced mixer, continues 40 ~ 60s of stirring；It will
Polypropylene fibre, cellulose ether, high-efficiency water-reducing agent of poly-carboxylic acid and nucleus type early strength agent are dispersed in water and form mixing water,
The mixing water of gross mass 80% is slowly injected into 20s in blender, marginal not enters side stirring 2min, then adds at once remaining total
The mixing water stirring 1min of quality 20% can discharge.
The beneficial effects of the invention are as follows：
The present invention is effectively utilized the waste liquid of the discarded rice husk of acid processing and production calcium lignosulfonate as raw material, not only energy saving
Environmental protection also reduces the production cost of hydrated calcium silicate early strength agent；Also, using the discarded rice husk of acid processing and production lignin
Hydrated calcium silicate early strength agent prepared by the waste liquid of sulfoacid calcium and the hydrated calcium silicate prepared using calcium sources such as calcium nitrate, calcium acetates are early
Strong agent similar nature can effectively improve the early strength and later strength of cement-based material.
Description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is the step flow chart of the preparation method of hydrated calcium silicate early strength agent silicon source of the present invention；
Fig. 2 is the step flow chart of the preparation method of hydrated calcium silicate early strength agent of the present invention.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates the basic structure of the present invention, therefore it only shows composition related to the present invention.
[embodiment 1]
As shown in Figure 1, 2, a kind of preparation method of hydrated calcium silicate early strength agent, this method include the following steps：
Obtain silicon source：
（1）Rice husk is selected to clean rice husk repeatedly with distilled water 3 ~ 5 times as silicon source；
（2）Rice husk after cleaning in 0.5 ~ 1mol/L hydrochloric acid solutions is impregnated into 12 ~ 48 h, cleans rice husk repeatedly until solution
It is filtered out after being in neutrality；
（3）Step will be passed through（2）Rice husk after cleaning is placed in 100 DEG C of air dry oven dry 24 h；
（4）Step will be passed through（3）The rice husk of acidizing pretreatment is placed in chamber type electric resistance furnace, with 10 DEG C/min heating rates from 25
It is taken out after DEG C being warming up to 400 ~ 800 DEG C of roasting 1h, grinding obtains white rice hull ash；
Rice husk fully burns in the oxidation environment of 400~800 DEG C, especially 400~800 DEG C, and rice hull ash carbon content is less, than
Surface area is larger, stable quality；Temperature is too low, and burning is insufficient, and rice hull ash carbon content is higher, and particle surface aperture becomes smaller, instead
Answer speed slow, yield reduces, filtration difficulty；Temperature is excessively high, grey carbon content and varying aperture unobvious, to furnace design
It is more demanding, while also excessively consume the energy.
（5）It is 1 in mass ratio by 0.5 ~ 1mol/L NaOH solutions and rice hull ash：2 ~ 3 input retort, at 40 ~ 80 DEG C
0.5 ~ 2h is reacted, after reaction, obtains silicon source after vacuum filtration；
Reactional equation：SiO2+ 2NaOH= Na2SiO3+ H2O
Influence of the reaction temperature to reaction speed is more apparent, considers reaction speed and energy saving two factors, will be warm
Degree control is preferably 60 DEG C or so, not only energy saving but also do not influence reaction speed at 40 ~ 80 DEG C.
Obtain calcium source：
（6）The waste liquid of production calcium lignosulfonate is selected as calcium source；
The preparation of ultra-pure water：
（7）Common water source is gone successively by more medium filter, active carbon filter, accurate filter, reverse osmosis equipment, electricity
Ion device, ultrapure water tank, ultrapure water pump and postposition cartridge filter, obtain deionized water；
（8）By step（7）In deionized water obtained boil 10 ~ 30min of heating, and nitrogen is passed through into water during heating
Gas obtains ultra-pure water, and the ultra-pure water prepared is detected using CO-2 analyser in water, makes the dense of carbon dioxide in water
Degree is less than 100ppm；
Because solubility is extremely low in water for nitrogen, after discharging carbon dioxide, continue heating.
Add in gel dispersal agent：
（9）Using the cetyl trimethylammonium bromide of cationic surfactant（CTAB）With the inorganic salts with cyclic structure
Calgon（SHMP）Compounding is used as gel dispersal agent, wherein, the additive amount ratio of CTAB and SHMP are 4:6, using light splitting
The absorbance of solution under photometer test different situations judges the dispersion effect of solution with this；
Hydrated calcium silicate particle has very high specific surface area and surface energy, and surface atom or number of ions are also very high, and surface is lived
Property increase, the attraction increase between particle is easily reunited between powder, and appearance impurity presence and surface defect and
Dangling bonds can also aggravate agglomeration, in order to make the uniform unlikely precipitation in the solution that suspends of the hydrated calcium silicate of generation, need
Disperseed with gelling dispersant.
Hydration calcium silicate powder surface is negative electrical charge, therefore is suitble to select the cetyl front three of cationic surfactant
Base ammonium bromide（CTAB）With the inorganic salts calgon with cyclic structure（SHMP）Compounding does modification to powder surface.
CTAB has longer hydrocarbon chain structure, and dispersion effect is derived from its absorption on powder surface, significantly enhances between particle
Repulsive interaction energy；SHMP is the inorganic salts for having cyclic structure, it is by improving particle surface current potential absolute value so as to produce
Raw strong electric double layer electrostatic repulsion forces disperse particle, meanwhile, SHMP can also enhance wetting journey of the particle surface to absolute ethyl alcohol
Degree, so as to prevent the reunion of particle.
The pattern of hydrated calcium silicate crystal is mainly fibrous structure, and after adulterating polyacrylamide, hydrated calcium silicate
Graininess is presented in pattern, and the dispersion of particle is evenly.
The absorbance of powder solution under different situations is tested using spectrophotometer, the dispersion effect of powder is judged with this；
The principle of powder dispersion effect is characterized using absorbance is：Substance is to extinction object in the absorbance and liquid phase medium of single wavelength light
The concentration of matter is directly proportional, i.e. the concentration of substance is higher, and absorbance is bigger.So absorbance is bigger in a dispersion medium for crystal,
Its dispersion performance is better.
It by taking hydrated calcium silicate as an example, is measured through overtesting, the additive amount ratio of CTAB and SHMP are 4:When 6, it can reach
Best dispersion effect, at this point, its absorbance value >=1.5.
Obtain hydrated calcium silicate early strength agent：
（10）In step（8）In in obtained ultra-pure water while be put into step（5）In silicon source and step obtained（6）Middle acquisition
The mass ratio of calcium source, wherein calcium source and silicon source is 1.0 ~ 1.7, and ultra-pure water is 9 ~ 12 with the mass ratio of silicon source and calcium source, is added simultaneously
Entering gel dispersal agent and polyacrylamide uniformly disperses reagent, prepares early strength agent using 60 DEG C of water bath with thermostatic control synthetic methods, instead
It answers period timing agitation and keeps solution ph more than 12；
（11）60 DEG C are heated to using temperature control magnetic stirring apparatus, carries out constant temperature multi-step mixing, 0 ~ 2h of phase keeps magnetic force before the reaction
Agitator speed makes reaction raw materials be sufficiently mixed uniformly in 200 ~ 300rpm；2 ~ 10h of phase keeps magnetic stirring apparatus to turn in the reaction
Speed improves reaction rate in 800 ~ 1000 rpm, holding higher rotation speed, and react fully completion；React 10 ~ 12h of later stage holding magnetic
Power agitator speed is in 200 ~ 300rpm so that reaction product uniformly disperses in aqueous solution；
（12）By step（11）The sample of middle acquisition is put into 60 DEG C of waters bath with thermostatic control and conserves, and curing age 7d will arrive age
Sample, which takes out, to be filtered, and filtrate carries out secondary suction filtration, and filter residue is poured into beaker, in magnetic stirring apparatus with 60 DEG C of deionized waters repeatedly
Washing, removes extra magazine and the complete sample of unreacted, filter residue is placed in 40 DEG C of vacuum drying chambers and is dried to constant weight,
It is put into and has kept dry in CaO drying vessel；
（13）Hydrated calcium silicate product of the particle diameter distribution between 50 ~ 200nm is detected, wherein grain size is selected to be in 100 ~ 150nm
Between hydrated calcium silicate product, obtain hydrated calcium silicate early strength agent.
According to the non-evaporating foster C30 self-compacting concretes of the early strength agent of type containing nucleus made from above-mentioned preparation method, 1m3Coagulation
In soil comprising 250Kg Portland cements 42.5,75Kg flyash, 750Kg sand, 290Kg handstones, the big stones of 760Kg,
150Kg water, polypropylene fibre, 25.2g cellulose ethers, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and the gel that quality volume is 0.1%
Quality of materials percentage is 10 ~ 15% nucleus type early strength agent；
The preparation method of the self-compacting concrete is：
Using forced mixer, wet-mixing after first dry mixing first adds in big stone, handstone and sand, starts forced mixer, stirs
Mix 40 ~ 60s；Portland cement 42.5 and flyash are added, starts forced mixer, continues 40 ~ 60s of stirring；It will
Polypropylene fibre, cellulose ether, high-efficiency water-reducing agent of poly-carboxylic acid and nucleus type early strength agent are dispersed in water and form mixing water,
The mixing water of gross mass 80% is slowly injected into 20s in blender, marginal not enters side stirring 2min, then adds at once remaining total
The mixing water stirring 1min of quality 20% can discharge.
[comparative example 1]
The difference of this comparative example and embodiment 1 is only that silicon source is conventional acquisition modes.
[comparative example 2]
The difference of this comparative example and embodiment 1 is only that calcium source is conventional acquisition modes.
[comparative example 3]
The difference of this comparative example and embodiment 1 is only using conventional deionized water.
[comparative example 4]
The difference of this comparative example and embodiment 1 is only without using dispersant.
[comparative example 5]
It is convention stir that the difference of this comparative example and embodiment 1, which is only agitating mode, without multi-step mixing.
[comparative example 6]
The difference of this comparative example and embodiment 1 is only to be screened without grain size.
[comparative example 7]
The difference of this comparative example and embodiment 1 is only that suction filtration mode is filtered to be conventional, without secondary suction filtration.
Compared with prior art, the present invention is effectively utilized the discarded rice husk of acid processing and produces the useless of calcium lignosulfonate
Liquid is as raw material, not only energy conservation and environmental protection, also reduces the production cost of hydrated calcium silicate early strength agent；It is also, useless using acid processing
It abandons rice husk and produces the hydrated calcium silicate early strength agent of the waste liquid preparation of calcium lignosulfonate and use sodium metasilicate as silicon source, nitric acid
Calcium, calcium acetate etc. are compared for hydrated calcium silicate early strength agent prepared by calcium source, and performance is more preferable, can effectively improve the morning of cement-based material
Phase intensity and later strength.
It is mixed the result shows that self-compaction can be significantly improved by the hydrated calcium silicate early strength agent that the preparation method of the present invention obtains
The early strength of soil is coagulated, as shown in table 1.
The intensity test result of 1 self-compacting concrete of table
| Number | 1d | 2d | 3d | 28d |
| Embodiment 1 | 12.6MPa | 20.2MPa | 24.3MPa | 36.8MPa |
| Comparative example 1 | 11.5MPa | 18.3MPa | 20.3MPa | 33.3MPa |
| Comparative example 2 | 11.8MPa | 19.2MPa | 21.6MPa | 34.5MPa |
| Comparative example 3 | 12.0MPa | 18.6MPa | 21.9MPa | 34.9MPa |
| Comparative example 4 | 10.8MPa | 17.8MPa | 20.8MPa | 30.6MPa |
| Comparative example 5 | 11.9MPa | 18.9MPa | 22.3MPa | 35.1MPa |
| Comparative example 6 | 10.9MPa | 17.6MPa | 20.6MPa | 30.4MPa |
| Comparative example 7 | 11.3MPa | 18.8MPa | 22.6MPa | 34.6MPa |
By the test of the contrast properties of comparative example and embodiment, it can be seen that, the concrete prepared using early strength agent of the present invention is in phase
With having higher intensity in the time, the early strength and later strength of concrete are higher than the prior art, thus the present invention
There is significant progress relative to the prior art.
Using above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the content on specification, it is necessary to determine its technical scope according to right.
Claims (10)
1. a kind of preparation method of hydrated calcium silicate early strength agent, it is characterised in that：This method includes the following steps：
（1）Obtain silicon source；
（2）Obtain calcium source；
（3）Calcium source and silicon source are mixed in ultra-pure water, gel dispersal agent is added in and polyacrylamide is uniformly dispersed, keep pH value of solution
Value is more than 12, and constant temperature multi-step mixing filters drying, hydrated calcium silicate early strength agent is obtained after screening after complete reaction.
2. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（1）Middle acquisition silicon source includes the following steps：
（1.1）Rice husk is selected to clean rice husk repeatedly with distilled water 3 ~ 5 times as silicon source；
（1.2）Step will be passed through（1.1）Rice husk after cleaning impregnates 12 ~ 48 h in 0.5 ~ 1mol/L hydrochloric acid solutions, with steaming
Distilled water cleans rice husk repeatedly until solution filters out after being in neutrality；
（1.3）Step will be passed through（1.2）Rice husk after cleaning is placed in 100 DEG C of air dry oven dry 24 h；
（1.4）The rice husk of above-mentioned acidizing pretreatment is placed in chamber type electric resistance furnace, with 10 DEG C/min heating rates from room temperature
It is taken out after to 400 ~ 800 DEG C of roasting 1h, grinding obtains white rice hull ash；
（1.5）It is 1 in mass ratio by 0.5 ~ 1mol/L NaOH solutions and rice hull ash：2 ~ 3 input retort, it is anti-at 40 ~ 80 DEG C
Answer 0.5 ~ 2h, after reaction, obtain silicon source after vacuum filtration.
3. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（2）Middle acquisition calcium source includes the following steps：
The waste liquid of production calcium lignosulfonate is selected as calcium source.
4. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（3）Described in the preparation method of ultra-pure water be：
Deionized water is boiled into 10 ~ 30min of heating, and nitrogen is passed through into water during heating, obtains ultra-pure water, it will
The ultra-pure water prepared is detected using CO-2 analyser, and the concentration of carbon dioxide in water is made to be less than 100ppm.
5. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（3）Described in the preparation method of gel dispersal agent be：
Using the cetyl trimethylammonium bromide of cationic surfactant（CTAB）With the inorganic salts six with cyclic structure
Sodium metaphosphate（SHMP）Compounding is used as gel dispersal agent, wherein, the additive amount ratio of CTAB and SHMP are 4:6, using light splitting light
The absorbance of solution under degree measurement examination different situations judges the dispersion effect of solution with this.
6. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（3）Middle multi-step mixing step is：60 DEG C are heated to using temperature control magnetic stirring apparatus, carries out constant temperature multi-step mixing；
0 ~ 2h of phase keeps magnetic stirring apparatus rotating speed reaction raw materials to be made to be sufficiently mixed uniformly in 200 ~ 300rpm before the reaction；
2 ~ 10h of phase holding magnetic stirring apparatus rotating speeds improve reaction rate in 800 ~ 1000rpm, holding higher rotation speed in the reaction,
React fully completion；
10 ~ 12h of phase keeps magnetic stirring apparatus rotating speed in 200 ~ 300rpm after the reaction so that reaction product is dispersed in water-soluble
In liquid.
7. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：The step
（3）It is middle to filter dry step and be：
Solution after above-mentioned constant temperature stepwise reaction is filtered, after suction filtration, filter residue is poured into beaker, and filtrate carries out
Secondary suction filtration washs filter residue with ultra-pure water repeatedly, removes undesired impurities and the complete sample of unreacted, filter residue is placed in 40 DEG C
It is dried in vacuum drying chamber to constant weight, is put into and has kept dry in CaO drying vessel.
8. a kind of preparation method of hydrated calcium silicate early strength agent according to claim 1, it is characterised in that：Step（3）In
Screening step is：Sample sifter is selected as precentagewise：Sample of the grain size less than 50nm accounts for gross sample 5 ~ 10%, and 50 ~ 200nm accounts for 80 ~
85%, surplus is more than 200nm.
9. one kind be added with the hydrated calcium silicate early strength agent that is prepared using the method described in any one of claim 1 ~ 8 from close
Real concrete, it is characterised in that：The hydrated calcium silicate early strength agent is applied to C30 self-compacting concretes, wherein：1m3Coagulation
In soil comprising 250Kg Portland cements 42.5,75Kg flyash, 750Kg sand, 290Kg handstones, the big stones of 760Kg,
150Kg water, polypropylene fibre, 25.2g cellulose ethers, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and the gelling that quality volume is 0.1%
Quality of materials percentage is 10 ~ 15% nucleus type early strength agent.
10. self-compacting concrete according to claim 9, it is characterised in that：The preparation method of the self-compacting concrete
For：
Using forced mixer, wet-mixing after first dry mixing first adds in big stone, handstone and sand, starts forced mixer, stirs
Mix 40 ~ 60s；Portland cement 42.5 and flyash are added, starts forced mixer, continues 40 ~ 60s of stirring；It will
Polypropylene fibre, cellulose ether, high-efficiency water-reducing agent of poly-carboxylic acid and nucleus type early strength agent are dispersed in water and form mixing water,
The mixing water of gross mass 80% is slowly injected into 20s in blender, marginal not enters side stirring 2min, then adds at once remaining total
The mixing water stirring 1min of quality 20% can discharge.
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| CN112661164A (en) * | 2020-12-22 | 2021-04-16 | 东南大学 | Method for preparing calcium silicate hydrate by using waste liquid as raw material |
| CN114656191A (en) * | 2022-04-28 | 2022-06-24 | 江苏博拓新型建筑材料股份有限公司 | Method for preparing crystal nucleus early-strength polycarboxylate superplasticizer with long-term dispersibility |
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