CN108249806B - 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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- CN108249806B CN108249806B CN201711331837.4A CN201711331837A CN108249806B CN 108249806 B CN108249806 B CN 108249806B CN 201711331837 A CN201711331837 A CN 201711331837A CN 108249806 B CN108249806 B CN 108249806B
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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
-
- 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
-
- 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
-
- 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
Abstract
The present invention relates to a kind of preparation methods of hydrated calcium silicate early strength agent, and using non-evaporating feeding C30 self-compacting concrete prepared by the early strength agent；It is effectively utilized acid and handles the waste liquid for discarding rice husk and production calcium lignosulfonate as raw material, not only energy conservation and environmental protection, also reduces the production cost of hydrated calcium silicate early strength agent；And, discarded rice husk is handled using acid and produces the hydrated calcium silicate early strength agent of the waste liquid preparation of calcium lignosulfonate and using silicon sources such as sodium metasilicate and using the hydrated calcium silicate early strength agent similar performance of the calcium sources such as calcium nitrate preparation, can effectively improve the early strength and later strength of cement-based material.
Description
Technical field
The present invention relates to the preparation methods and use of the field of building materials more particularly to a kind of hydrated calcium silicate early strength agent should
The self-compacting concrete of early strength agent.
Background technique
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 demoulding of precast concrete with this
Between.And primary product of the hydrated calcium silicate as hydrated cementitious, it is used as early strength agent, 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 that hydrated cementitious speed is improved, to mention
The early strength of high cement-based material.
Currently, the preparation method of hydrated calcium silicate mainly has hydro-thermal method and chemical coprecipitation.Hydro-thermal method prepares aquation silicon
When sour calcium, temperature-pressure is needed, energy consumption is high when production, and hydrated calcium silicate partial size obtained is larger, specific surface area is smaller, unfavorable
In the early strength for improving hydrated calcium silicate；And chemical coprecipitation has the advantages that simple process, low energy consumption, can be avoided height
The working environment of warm high pressure, but when preparing hydrated calcium silicate using chemical coprecipitation, silicon source used is the silicon salts such as sodium metasilicate,
Calcium source used is the calcium salts such as calcium nitrate, calcium acetate or calcium chloride, these silicon salt calcium salt prices are higher, increase hydrated calcium silicate
Production cost.
It is rich in silicon salt in the rice husk discarded after grain harvest, silicon salt acid dissolution therein can be used 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 the calcium source for preparing 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.
Summary of the invention
The technical problem to be solved by the present invention is currently, the preparation method of hydrated calcium silicate mainly has hydro-thermal method and chemistry
Coprecipitation, hydro-thermal method need temperature-pressure, and production energy consumption is high, and are unfavorable for improving the early strong effect of hydrated calcium silicate；And change
Learning silicon source used in coprecipitation is the silicon salts such as sodium metasilicate, and calcium source is the calcium salts such as calcium nitrate, calcium acetate or calcium chloride, these silicon salts and
Calcium salt price is higher, increases the production cost of hydrated calcium silicate；Lack less energy consumption in the prior art and can make profits again simultaneously
The method for preparing hydrated calcium silicate early strength agent 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: method includes the following steps:
(1) silicon source is obtained；
(2) calcium source is obtained；
(3) calcium source and silicon source are mixed in ultrapure water, and gel dispersal agent is added and polyacrylamide is uniformly dispersed, keeps molten
Liquid pH value is greater than 12, and constant temperature multi-step mixing filters drying after complete reaction, hydrated calcium silicate early strength agent is obtained after screening.
Further, obtain silicon source in step (1) the following steps are included:
(1.1) it selects rice husk as silicon source, rice husk is cleaned 3 ~ 5 times repeatedly with distilled water；
(1.2) rice husk after step (1.1) are cleaned is impregnated into 12 ~ 48 h in 0.5 ~ 1mol/L hydrochloric acid solution,
Rice husk is cleaned repeatedly with distilled water until solution filters out after being in neutrality；
(1.3) rice husk after step (1.2) cleaning is placed in 100 DEG C of air dry oven dry 24 h；
(1.4) rice husk of above-mentioned acidizing pretreatment is placed in chamber type electric resistance furnace, with 10 DEG C/min heating rate from room temperature
It is taken out after being warming up to 400 ~ 800 DEG C of 1 h of roasting, grinding obtains white rice hull ash；
It (1.5) is in mass ratio that 1:2 ~ 3 puts into reactor tank by 0.5 ~ 1mol/L NaOH solution and rice hull ash, at 40 ~ 80 DEG C
0.5 ~ 2h of lower reaction obtains silicon source after reaction after vacuum filtration.
Further, obtain calcium source in step (2) the following steps are included:
Select the waste liquid of production calcium lignosulfonate as calcium source.
Further, ultrapure water described in step (3) the preparation method comprises the following steps:
Deionized water is boiled into 10 ~ 30min of heating, and is passed through nitrogen into water during heating, is obtained ultrapure
The ultrapure water prepared is detected using CO-2 analyser, makes the concentration of carbon dioxide in water lower than 100ppm by water.
Further, gel dispersal agent described in step (3) the preparation method comprises the following steps:
Using the cetyl trimethylammonium bromide (CTAB) of cationic surfactant and with the inorganic of cyclic structure
Salt calgon (SHMP) compounding be used as gel dispersal agent, wherein the additive amount ratio of CTAB and SHMP be 4:6, using point
Light photometer tests the absorbance of solution under different situations, and the dispersion effect of solution is judged with this.
Further, multi-step mixing step in step (3) are as follows: be heated to 60 DEG C using temperature control magnetic stirring apparatus, carry out permanent
Warm multi-step mixing；
0 ~ 2h of phase keeps magnetic stirring apparatus revolving speed in 200 ~ 300rpm before the reaction, is sufficiently mixed reaction raw materials uniformly；
2 ~ 10h of phase keeps magnetic stirring apparatus revolving speed in 800 ~ 1000rpm in the reaction, and higher rotation speed is kept to improve reaction speed
Rate, react fully completion；
10 ~ 12h of phase keeps magnetic stirring apparatus revolving speed in 200 ~ 300rpm after the reaction, so that reaction product is dispersed in
In aqueous solution.
Further, dry step is filtered in step (3) are as follows:
Solution after above-mentioned constant temperature stepwise reaction is filtered, after suction filtration, filter residue is poured into beaker, filtrate
Secondary suction filtration is carried out, filter residue is washed repeatedly with ultrapure water, undesired impurities and the complete sample of unreacted is removed, filter residue is placed in
It is dried in 40 DEG C of vacuum ovens to constant weight, is put into and has kept dry in the dry vessel of CaO.
Further, screening step in step (3) are as follows: sample sifter is selected as precentagewise: partial size is less than the sample of 50nm
Gross sample 5 ~ 10% is accounted for, 50 ~ 200nm accounts for 80 ~ 85%, and surplus is 200nm or more.
Further, the present invention also provides it is a kind of added with using the above method preparation hydrated calcium silicate early strength agent from
Hydrated calcium silicate early strength agent is applied to C30 self-compacting concrete, in which: 1m by air-free concrete3It include 250Kg in concrete
Ordinary portland cement 42.5,75Kg flyash, 750Kg sand, 290Kg handstone, the big stone of 760Kg, 150Kg water, quality are mixed
Polypropylene fibre, 25.2g cellulose ether, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and the cementitious material mass percent that amount is 0.1%
For 10 ~ 15% nucleus type early strength agent.
Further, self-compacting concrete the preparation method comprises the following steps:
Using forced mixer, big stone, handstone and sand is first added in wet-mixing after first dry mixing, starts forced action type stirring
Machine stirs 40 ~ 60s；Add ordinary portland cement 42.5 and flyash, start forced mixer, continue stirring 40 ~
60s；Polypropylene fibre, cellulose ether, high-efficiency water-reducing agent of poly-carboxylic acid and nucleus type early strength agent are dispersed in be formed in water and mixed
Heshui is slowly injected into the mixing water of gross mass 80% in 20s in blender, and marginal not enters side stirring 2min, is then added at once surplus
The mixing water stirring 1min of remaining gross mass 20% can discharge.
The beneficial effects of the present invention are:
The present invention is effectively utilized acid and handles the waste liquid for discarding rice husk and production calcium lignosulfonate as raw material, not only
Energy conservation and environmental protection also reduces the production cost of hydrated calcium silicate early strength agent；Also, discarded rice husk and production wood are handled using acid
The hydrated calcium silicate early strength agent of the waste liquid preparation of quality sulfoacid calcium and the aquation silicic acid prepared using the calcium sources such as calcium nitrate, calcium acetate
Calcium early strength agent similar performance can effectively improve the early strength and later strength of cement-based material.
Detailed description of the invention
Present invention will be further explained below with reference to the attached 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 basic structure of the invention, therefore it only shows the composition relevant to the invention.
[embodiment 1]
As shown in Figure 1, 2, a kind of preparation method of hydrated calcium silicate early strength agent, method includes the following steps:
Obtain silicon source:
(1) it selects rice husk as silicon source, rice husk is cleaned 3 ~ 5 times repeatedly with distilled water；
(2) will clean after rice husk impregnates 12 ~ 48 h in 0.5 ~ 1mol/L hydrochloric acid solution, repeatedly clean rice husk up to
Solution filters out after being in neutrality；
(3) rice husk after step (2) cleaning is placed in 100 DEG C of air dry oven dry 24 h；
(4) it will be placed in chamber type electric resistance furnace by the rice husk of step (3) acidizing pretreatment, with 10 DEG C/min heating rate
From 25 DEG C be warming up to 400 ~ 800 DEG C of roasting 1h after take out, grinding obtain white rice hull ash；
Rice husk full combustion in the oxidation environment of 400~800 DEG C, especially 400~800 DEG C, rice hull ash carbon content compared with
Few, specific surface area is larger, and quality is stablized；Temperature is too low, burns insufficient, and rice hull ash carbon content is higher, and particle surface aperture becomes
Small, reaction speed is slow, and yield reduces, filtration difficulty；Temperature is excessively high, and grey carbon content and varying aperture are unobvious, to burning
Furnace design requirement is higher, while also excessively consuming the energy.
It (5) is in mass ratio that 1:2 ~ 3 puts into reactor tank by 0.5 ~ 1mol/L NaOH solution and rice hull ash, at 40 ~ 80 DEG C
0.5 ~ 2h of reaction obtains silicon source after reaction after vacuum filtration；
Reactional equation: SiO2+ 2NaOH= Na2SiO3+ H2O
Influence of the reaction temperature to reaction speed is more obvious, comprehensively considers reaction speed and energy saving two factors,
Temperature is controlled at 40 ~ 80 DEG C, it is preferably 60 DEG C or so, not only energy saving but also do not influence reaction speed.
Obtain calcium source:
(6) select the waste liquid of production calcium lignosulfonate as calcium source；
The preparation of ultrapure water:
(7) by common water source successively pass through more medium filter, active carbon filter, accurate filter, reverse osmosis equipment,
Electric deion equipment, ultrapure water tank, ultrapure water pump and postposition cartridge filter, obtain deionized water；
(8) deionized water obtained in step (7) is boiled into 10 ~ 30min of heating, and led to during heating into water
Enter nitrogen, obtain ultrapure water, the ultrapure water prepared is detected using CO-2 analyser in water, makes carbon dioxide in water
Concentration be lower than 100ppm；
Because solubility is extremely low in water for nitrogen, after carbon dioxide is discharged, continue heating.
Gel dispersal agent is added:
(9) using the cetyl trimethylammonium bromide (CTAB) of cationic surfactant and the nothing with cyclic structure
Machine salt calgon (SHMP) compounding is used as gel dispersal agent, wherein the additive amount ratio of CTAB and SHMP is 4:6, is used
Spectrophotometer tests the absorbance of solution under different situations, and the dispersion effect of solution is judged 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, table
Face activity increases, and the attraction between particle increases, and easily reunites between powder, and appearance impurity presence and surface lack
It falls into and dangling bonds can also aggravate agglomeration, in order to make the hydrated calcium silicate generated uniformly suspend unlikely precipitating in the solution,
It needs to be dispersed with gelling dispersing agent.
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) and with cyclic structure inorganic salts calgon (SHMP) compounding modification is done 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 with cyclic structure, it is by improving particle surface current potential absolute value to produce
Raw strong electric double layer electrostatic repulsion forces disperse particle, meanwhile, particle surface also can be enhanced to the wetting journey of dehydrated alcohol in SHMP
Degree, 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 more evenly.
The absorbance that powder solution under different situations is tested using spectrophotometer, the dispersion effect of powder is judged with this；
Principle using absorbance characterization powder dispersion effect 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, measures through overtesting, when the additive amount ratio of CTAB and SHMP are 4:6, can achieve
Optimal dispersion effect, at this point, its absorbance value >=1.5.
Obtain hydrated calcium silicate early strength agent:
(10) it is put into step (5) in the ultrapure water obtained in step (8) and is obtained in silicon source obtained and step (6) simultaneously
The calcium source obtained, wherein the mass ratio of calcium source and silicon source is 1.0 ~ 1.7, and ultrapure water is 9 ~ 12 with the mass ratio of silicon source and calcium source, together
When gel dispersal agent and polyacrylamide be added keep reagent evenly dispersed, prepared using 60 DEG C of water bath with thermostatic control synthetic methods early strong
Agent timing agitation and keeps solution ph 12 or more during reaction；
(11) 60 DEG C are heated to using temperature control magnetic stirring apparatus, carry out constant temperature multi-step mixing, 0 ~ 2h of phase is kept before the reaction
Magnetic stirring apparatus revolving speed is sufficiently mixed reaction raw materials uniformly in 200 ~ 300rpm；2 ~ 10h of phase keeps magnetic agitation in the reaction
Device revolving speed keeps higher rotation speed to improve reaction rate, react fully completion in 800 ~ 1000 rpm；10 ~ 12h of later period is reacted to protect
Magnetic stirring apparatus revolving speed is held in 200 ~ 300rpm, so that reaction product is evenly dispersed in aqueous solution；
(12) sample obtained in step (11) is put into 60 DEG C of waters bath with thermostatic control and is conserved, curing age 7d will be to age
The sample of phase, which takes out, to be filtered, and filtrate carries out secondary suction filtration, and filter residue pours into beaker, with 60 DEG C of deionized waters in magnetic stirring apparatus
Wash repeatedly, remove extra magazine and the complete sample of unreacted, filter residue is placed in 40 DEG C of vacuum ovens be dried to
Constant weight is put into and has kept dry in the dry vessel of CaO；
(13) hydrated calcium silicate product of the detection particle diameter distribution between 50 ~ 200nm, selection wherein partial size be in 100 ~
Hydrated calcium silicate product between 150nm, obtains hydrated calcium silicate early strength agent.
According to the non-evaporating feeding C30 self-compacting concrete of the early strength agent of type containing nucleus made from above-mentioned preparation method, 1m3Coagulation
In soil comprising 250Kg ordinary portland cement 42.5,75Kg flyash, 750Kg sand, 290Kg handstone, the big stone of 760Kg,
150Kg water, polypropylene fibre, 25.2g cellulose ether, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and the gel that quality volume is 0.1%
The nucleus type early strength agent that quality of materials percentage is 10 ~ 15%；
The self-compacting concrete the preparation method comprises the following steps:
Using forced mixer, big stone, handstone and sand is first added in wet-mixing after first dry mixing, starts forced action type stirring
Machine stirs 40 ~ 60s；Add ordinary portland cement 42.5 and flyash, start forced mixer, continue stirring 40 ~
60s；Polypropylene fibre, cellulose ether, high-efficiency water-reducing agent of poly-carboxylic acid and nucleus type early strength agent are dispersed in be formed in water and mixed
Heshui is slowly injected into the mixing water of gross mass 80% in 20s in blender, and marginal not enters side stirring 2min, is then added at once surplus
The mixing water stirring 1min of remaining gross mass 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 not use dispersing agent.
[comparative example 5]
The difference of this comparative example and embodiment 1 is only that agitating mode is convention stir, without multi-step mixing.
[comparative example 6]
The difference of this comparative example and embodiment 1 is only to screen without partial size.
[comparative example 7]
The difference of this comparative example and embodiment 1 is only that suction filtration mode filters to be conventional, without secondary suction filtration.
Compared with prior art, the present invention is effectively utilized acid and handles discarded rice husk and produce the useless of calcium lignosulfonate
Liquid is as raw material, and not only energy conservation and environmental protection, also reduces the production cost of hydrated calcium silicate early strength agent；Also, it is 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 for silicon source, nitric acid
Calcium, calcium acetate etc. are that the hydrated calcium silicate early strength agent of calcium source preparation is compared, 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 the hydrated calcium silicate early strength agent that preparation method through the invention obtains can significantly improve self-compaction
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 |
It can see by the test of the contrast properties of comparative example and embodiment, the concrete prepared using early strength agent of the present invention
There is higher intensity in the same time, the early strength and later strength of concrete are higher than the prior art, thus this
Invention has significant progress compared with the existing technology.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above 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 contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (2)
1. a kind of preparation method of hydrated calcium silicate early strength agent, it is characterised in that: method includes the following steps:
(1) silicon source is obtained；
(2) calcium source is obtained；
(3) calcium source and silicon source are mixed in ultrapure water, and gel dispersal agent is added and polyacrylamide is uniformly dispersed, keeps pH value of solution
Value is greater than 12, and constant temperature multi-step mixing filters drying after complete reaction, hydrated calcium silicate early strength agent is obtained after screening；
Silicon source is obtained in the step (1) the following steps are included:
(1.1) it selects rice husk as silicon source, rice husk is cleaned 3 ~ 5 times repeatedly with distilled water；
(1.2) rice husk after step (1.1) are cleaned is impregnated into 12 ~ 48 h in 0.5 ~ 1mol/L hydrochloric acid solution, with steaming
Distilled water cleans rice husk repeatedly until solution filters out after being in neutrality；
(1.3) rice husk after step (1.2) cleaning is placed in 100 DEG C of air dry oven dry 24 h；
(1.4) rice husk of above-mentioned acidizing pretreatment is placed in chamber type electric resistance furnace, with 10 DEG C/min heating rate from room temperature
It is taken out after to 400 ~ 800 DEG C of roasting 1h, grinding obtains white rice hull ash；
It (1.5) is in mass ratio that 1:2 ~ 3 puts into reactor tank by 0.5 ~ 1mol/L NaOH solution and rice hull ash, it is anti-at 40 ~ 80 DEG C
Answer 0.5 ~ 2h, after reaction, obtain silicon source after vacuum filtration；
Calcium source is obtained in the step (2) the following steps are included: selecting the waste liquid of production calcium lignosulfonate as calcium source；
Ultrapure water described in the step (3) the preparation method comprises the following steps:
Deionized water is boiled into 10 ~ 30min of heating, and is passed through nitrogen into water during heating, obtains ultrapure water, it will
The ultrapure water prepared is detected using CO-2 analyser, makes the concentration of carbon dioxide in water lower than 100ppm；
Gel dispersal agent described in the step (3) the preparation method comprises the following steps:
Using cationic surfactant cetyl trimethylammonium bromide CTAB and the inclined phosphorus of the inorganic salts with cyclic structure six
Sour sodium SHMP compounding is used as gel dispersal agent, wherein the additive amount ratio of CTAB and SHMP is 4:6, is measured using spectrophotometric
The absorbance for trying solution under different situations, the dispersion effect of solution is judged with this；
Multi-step mixing step in the step (3) are as follows: be heated to 60 DEG C using temperature control magnetic stirring apparatus, carry out constant temperature substep and stir
It mixes；
0 ~ 2h of phase keeps magnetic stirring apparatus revolving speed in 200 ~ 300rpm before the reaction, is sufficiently mixed reaction raw materials uniformly；
2 ~ 10h of phase keeps magnetic stirring apparatus revolving speed in 800 ~ 1000rpm in the reaction, and higher rotation speed is kept to improve reaction rate,
React fully completion；
10 ~ 12h of phase keeps magnetic stirring apparatus revolving speed in 200 ~ 300rpm after the reaction so that reaction product be dispersed in it is water-soluble
In liquid；
Dry step is filtered in the step (3) are as follows:
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 ultrapure water repeatedly, removes undesired impurities and the complete sample of unreacted, filter residue is placed in 40 DEG C
It is dried in vacuum oven to constant weight, is put into and has kept dry in the dry vessel of CaO；
Screening step in the step (3) are as follows: sample sifter is divided into precentagewise: partial size less than 50nm sample account for gross sample 5 ~
10%, 50 ~ 200nm account for 80 ~ 85%, and surplus is 200nm or more.
2. a kind of self-compaction coagulation added with the hydrated calcium silicate early strength agent using the preparation of method described in claim 1
Soil, it is characterised in that: the hydrated calcium silicate early strength agent is applied to C30 self-compacting concrete, in which: 1m3It is wrapped in concrete
Ordinary portland cement containing 250Kg 42.5,75Kg flyash, 750Kg sand, 290Kg handstone, the big stone of 760Kg, 150Kg water,
Polypropylene fibre, 25.2g cellulose ether, 6.5Kg high-efficiency water-reducing agent of poly-carboxylic acid and the cementitious material quality that quality volume is 0.1%
The nucleus type early strength agent that percentage is 10 ~ 15%；
The self-compacting concrete the preparation method comprises the following steps:
Using forced mixer, wet-mixing after first dry mixing is first added big stone, handstone and sand, starts forced mixer, stirs
Mix 40 ~ 60s；Ordinary portland cement 42.5 and flyash are added, forced mixer is started, 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, is then added at once remaining total
The mixing water stirring 1min of quality 20% can discharge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711331837.4A CN108249806B (en) | 2017-12-13 | 2017-12-13 | A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711331837.4A CN108249806B (en) | 2017-12-13 | 2017-12-13 | A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete |
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| Publication Number | Publication Date |
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| CN108249806A CN108249806A (en) | 2018-07-06 |
| CN108249806B true CN108249806B (en) | 2019-10-01 |
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| CN109369055B (en) * | 2018-11-22 | 2022-01-21 | 中耕耘成建筑科技(江苏)有限公司 | Composite early strength agent and self-compacting concrete prepared by utilizing same |
| CN109369051A (en) * | 2018-11-22 | 2019-02-22 | 中耕耘成建筑科技(江苏)有限公司 | A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete |
| CN109665737B (en) * | 2018-12-17 | 2021-08-13 | 湖北工业大学 | Nano-set early strength water reducing agent for sulphoaluminate cement |
| CN109650398B (en) * | 2019-02-19 | 2020-07-17 | 科之杰新材料集团有限公司 | Calcium silicate hydrate early strength agent and preparation method thereof |
| CN110330257B (en) * | 2019-04-11 | 2021-09-14 | 武汉理工大学 | C-S-H gel nanocrystal core early strength agent and preparation method and application thereof |
| CN111170324A (en) * | 2020-01-21 | 2020-05-19 | 张战军 | Method for preparing light high-whiteness calcium silicate micro powder by using rice hull ash |
| CN111499306B (en) * | 2020-04-28 | 2021-12-28 | 安徽省高迪循环经济产业园股份有限公司 | Unfired fly ash ceramsite prefabricated ecological bank protection structure and preparation method thereof |
| CN111875313B (en) * | 2020-07-14 | 2022-06-03 | 华润水泥技术研发有限公司 | Preparation method of super early strength self-compacting concrete applied to PC (polycarbonate) member |
| CN111995272A (en) * | 2020-09-02 | 2020-11-27 | 中国地质大学（武汉） | Rice hull ash and preparation method thereof, rice hull ash geopolymer and preparation method thereof |
| CN112430003B (en) * | 2020-12-04 | 2022-05-31 | 盐城工学院 | Size-controllable nano composite early strength agent and preparation method thereof |
| 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 |
| CN114656191B (en) * | 2022-04-28 | 2023-03-17 | 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 |
| CN116040995A (en) * | 2023-01-06 | 2023-05-02 | 新旺基科技工程集团有限公司 | High-adhesion high-strength concrete for self-leveling terrace and preparation method |
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| CN104402288A (en) * | 2014-10-29 | 2015-03-11 | 上海建工集团股份有限公司 | Calcium silicate hydrate gel solution early strength agent and preparation method thereof |
| CN104891884A (en) * | 2015-05-20 | 2015-09-09 | 中民筑友有限公司 | C35 low-gel-material self-compacting concrete and preparation method thereof |
| CN105753000A (en) * | 2016-02-29 | 2016-07-13 | 同济大学 | Preparation method and application method of hydrated calcium silicate seed crystal |
| CN105777006A (en) * | 2016-03-14 | 2016-07-20 | 同济大学 | Non-steam autoclaved high performance concrete tube pile using calcium silicate hydrate seed powder as exciting agent, and preparation method of non-steam autoclaved high performance concrete tube pile |
| CN106630723B (en) * | 2016-10-11 | 2019-06-28 | 江苏苏博特新材料股份有限公司 | A kind of preparation method of concrete early strength agent |
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Address after: Jianke science and Technology Park, No.1, Xiangshan Avenue, Gaozi street, Zhenjiang City, Jiangsu Province Patentee after: ZHENJIANG JIANKE CONSTRUCTION TECHNOLOGY Co.,Ltd. Address before: Beijing Xian Road 212000 Zhenjiang city Jiangsu province Jingkou District No. 38 Patentee before: ZHENJIANG JIANKE CONSTRUCTION TECHNOLOGY Co.,Ltd. |