CN109734347A - A kind of enhanced alkali-free quick-coagulant of nanosized seeds and preparation method thereof - Google Patents
A kind of enhanced alkali-free quick-coagulant of nanosized seeds and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to enhanced alkali-free quick-coagulants of a kind of nanosized seeds and preparation method thereof, the accelerator is made of the raw material of following mass parts: lithium sulfate 0% ~ 15%, aluminum sulfate 30% ~ 50%, magnesium sulfate 5% ~ 10%, modified manometer silicon dioxide microballoon 5% ~ 15%, organic alcohol amine 5% ~ 10%, inorganic acid 3% ~ 5%, surplus are water.The enhanced alkali-free quick-coagulant of nanosized seeds provided by the present invention has the modified manometer silicon dioxide microballoon of parents characteristic by introducing, it is set to serve as nucleus in cement hydration process, to effectively improve the hydration rate of cement in gunite concrete, gunite concrete early stage and later strength are significantly improved.The novel alkali-free quick-coagulant has that volume is low, stability is good, the high outstanding features such as friendly with production environment of strength retention ratio, can effectively improve the mechanical property and endurance quality of gunite concrete.
Description
Technical field
The invention belongs to technical field of concrete additives, in particular to a kind of enhanced alkali-free quick-coagulant of nanosized seeds.
Background technique
Accelerator is that one kind can make concrete condense the additive of hardening rapidly, is mainly used for applying for gunite concrete
Work.Accelerator, which is divided into, two class of alkali accelerator and alkali-free quick-coagulant.Wherein, alkali accelerator refers to Na2O equivalent content is greater than
1.0% accelerator, such accelerator although can satisfy gunite concrete initial stage condensation hardening requirement, but due to
Its alkali content is higher, so that gunite concrete micro-structure is loose, causes it big, durability deficiency of later strength loss etc. occur and asks
Topic.Therefore, research and development alkali-free quick-coagulant has become the research hotspot in international accelerator field.
Currently, researchers at home and abroad have been carried out extensive exploration to alkali-free quick-coagulant, but wherein there are still problems.
Be mainly reflected in following three aspect: (1) alkali-free quick-coagulant alkali content in part is still higher.Come from presently disclosed accelerator patent
It sees, although entitled alkali-free quick-coagulant, alkali content is still higher in its real composition, such as Chinese patent CN106866017A " one
Kind alkali-free quick-coagulant and its product ", sodium fluoride mass fraction are 10 ~ 15%；For another example Chinese patent CN107857501A is " a kind of
Containing the alkali-free quick-coagulant and preparation method thereof for promoting solidifying early strength agent organic amine substance ", sodium fluoride mass fraction reaches as high as
15%；For another example Chinese patent CN107298540A " a kind of anti-freezing type alkali-free quick-coagulant and the preparation method and application thereof ", practical group
Divide containing sodium fluoride and best quality number is also up to 3%.These accelerators are not able to satisfy " the gunite concrete speed newly promulgated
Solidifying agent " alkali content should not exceed 1.0% requirement in (GB ∕ T 35159-2017).(2) part alkali-free quick-coagulant is difficult to coordinate to coagulate
Tie the contradiction between time and early strength.Alkali metal containing substance, the solidifying effect of rush do not have lower than traditional in alkali-free quick-coagulant
Alkali accelerator.It is required to meet setting time, people generally use the method for increasing alkali-free quick-coagulant volume come when shortening condensation
Between.If alkali-free quick-coagulant volume is up to the 10% of cement quality in Chinese patent CN1974466A, German BASF produces MEYCO
SA160 type accelerator suggests that volume is more up to the 11% of cement quality.Though higher accelerator volume can be shortened cement slurry/mixed
It coagulates the setting time of soil, but introduces the spatial network hole that the inorganic salts such as aluminum sulfate generate a large amount of entringite at hydrated cementitious initial stage
Dense packing effect is not obtained, cement slurry/concrete early strength will be significantly affected.(3) production of part alkali-free quick-coagulant
It has greater environmental impacts with using.Part alkali-free quick-coagulant uses hydrofluoric acid as stabilizer in existing patent, which makes
Although it is produced and use process will bring environment and Health Status For Workers Exposed with the stability for improving alkali-free quick-coagulant
Adverse effect.As the above analysis, a kind of high stable, early strong, later strength not retraction environmentally friendly alkali-free speed are researched and developed
Solidifying agent is of great significance to gunite concrete comprehensive performance is promoted.
Summary of the invention
The purpose of the invention is to overcome, traditional alkali-free quick-coagulant stability is poor, volume is high, early strength is insufficient, environment
The enhanced alkali-free quick-coagulant of a kind of nanosized seeds for influencing the deficiencies of big and proposing.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of enhanced alkali-free quick-coagulant of nanosized seeds includes the raw material of following mass parts: lithium sulfate 0% ~ 15%, and aluminum sulfate 30% ~
50%, magnesium sulfate 5% ~ 10%, modified manometer silicon dioxide microballoon 5% ~ 15%, organic alcohol amine 5% ~ 10%, inorganic acid 3% ~ 5%, surplus is
Water.
The lithium sulfate is commercially available technical grade sulfuric acid lithium.
The aluminum sulfate is commercially available technical grade sulfuric acid aluminium, wherein Al2O3Content is greater than 17%.
The magnesium sulfate is commercially available technical grade epsom salt, and wherein active constituent content is greater than 99%.
The modified manometer silicon dioxide microballoon is the accelerating component with parents characteristic, particle size be 50nm ~
100nm.The preparation process of the component is as follows: with polystyrene spheres (PS) for matrix, adsorption cetyl trimethyl bromination
Ammonium (CTAB), using the electrostatic interaction for the silicon species anion that CTAB cation and ethyl orthosilicate (TEOS) hydrolyze, by dioxy
SiClx is coated on PS ball, so that the nanometer titanium dioxide silicon seed reinforcing material be made.The material is in cement hydration process
Crystal seed is served as, the nucleation barrier of hydrolysis product of cement is effectively reduced, to accelerate the formation of hydrated product in concrete, fills calcium
The coarse pore that aluminite is formed, effectively improves early stage and the later strength of gunite concrete.
The organic alcohol amine is one of tetrahydroxyethyl-ethylene diamine, triisopropanolamine, triethanolamine or a variety of, is being heated
Organic alcohol amine forms the stabilizing network structure of space interpenetrating in whipping process, this is also that improved silica crystal seed can in the present invention
With the key of stable suspersion in the solution.Rate of addition and mixing speed are to ensure that an important factor for forming stabilizing network structure,
The time for adding of organic alcohol amine of the present invention is 0.5h ~ 1h, and mixing speed is the rpm of 300 rpm ~ 500.
The inorganic acid is one of citric acid, salicylic acid, phosphoric acid or a variety of, is carried out using inorganic acid to mixed solution
PH is adjusted, and can effectively promote stability of solution.The stabilization pH value range of alkali-free quick-coagulant of the present invention is 2.0 ~ 4.0.
A kind of preparation of the enhanced alkali-free quick-coagulant of nanosized seeds of the present invention, comprising the following steps:
Step 1: with polystyrene spheres (PS) for matrix, adsorption cetyl trimethylammonium bromide (CTAB) utilizes CTAB
The electrostatic interaction of cation and ethyl orthosilicate (TEOS) hydrolysis silicon matter anion, the coated with silica that hydrolysis obtains is existed
On PS ball, through filtering, cleaning and drying, the nano modification silicon dioxide microsphere is made, for use.
Step 2: lithium sulfate, aluminum sulfate and magnesium sulfate being mixed with water, are 60 DEG C ~ 80 DEG C, speed of agitator 300 in temperature
1h ~ 2h is reacted under conditions of the rpm of rpm ~ 500.
Step 3: keeping temperature and speed of agitator constant, organic alcohol amine is slowly added dropwise, guarantees at the uniform velocity to be added dropwise in 0.5h ~ 1h
It completes.
Step 4: keeping temperature and speed of agitator constant, be slowly added to inorganic acid, adjust mixed liquor pH value to 2.0 ~ 4.0.
Step 5: it is constant to be kept stirring revolving speed, and the addition of modified manometer silicon dioxide microballoon made from step 1 step 4 is obtained
Mixed liquor in, stir 0.5h ~ 1h, make its even suspension, be slowly cooled to room temperature, be made the enhanced alkali-free rapid hardening of nanosized seeds
Agent.
Specific embodiment
For a better understanding of the invention, the content of present invention is further described below with reference to embodiment, but the present invention
Content be not limited to the express ranges of embodiment.
Embodiment 1
The preparation of the enhanced alkali-free quick-coagulant of nanosized seeds, comprising the following steps:
(1) the nano silica microsphere material is prepared.
(2) 5g lithium sulfate, 40g aluminum sulfate, 6g magnesium sulfate are mixed with 36g distilled water, is stirred under 60 DEG C of water bath conditions
To whole dissolutions, mixing speed 300rpm.
(3) it keeps temperature and speed of agitator constant, 5g tetrahydroxyethyl-ethylene diamine is slowly added dropwise in the above solution, speed is added dropwise
Degree is 1.0 ml/min.
(4) 3g citric acid is slowly added in above-mentioned mixed solution and is stirred, adjust mixed solution pH value to 3.0.
(5) 5g nano silica microsphere material is added in mixed solution obtained by (4), under the conditions of 300 rpm of revolving speed
1h is stirred, makes its even suspension, so that the enhanced alkali-free quick-coagulant of nanosized seeds of the invention be made.
Embodiment 2
The preparation of the enhanced alkali-free quick-coagulant of nanosized seeds, comprising the following steps:
(1) the nano silica microsphere material is prepared.
(2) 40g aluminum sulfate, 8g magnesium sulfate are mixed with 36g distilled water, is stirred under 60 DEG C of water bath conditions to all molten
Solution, mixing speed 300rpm.
(3) it keeps temperature and speed of agitator constant, 5g triisopropanolamine is slowly added dropwise in the above solution, rate of addition is
1.0 ml/min。
(4) 3g citric acid is slowly added in above-mentioned mixed solution and is stirred, adjust mixed solution pH value to 3.0.
(5) 8g nano silica microsphere material is added in mixed solution obtained by (4), under the conditions of 300 rpm of revolving speed
1h is stirred, makes its even suspension, so that the enhanced alkali-free quick-coagulant of nanosized seeds of the invention be made.
Embodiment 3
The preparation of the enhanced alkali-free quick-coagulant of nanosized seeds, comprising the following steps:
(1) the nano silica microsphere material is prepared.
(2) 40g aluminum sulfate, 5g magnesium sulfate are mixed with 32g distilled water, is stirred under 60 DEG C of water bath conditions to all molten
Solution, mixing speed 300rpm.
(3) it keeps temperature and speed of agitator constant, 8g triethanolamine is slowly added dropwise in the above solution, rate of addition is
1.0 ml/min。
(4) 3g salicylic acid is slowly added in above-mentioned mixed solution and is stirred, adjust mixed solution pH value to 3.0.
(5) 12g nano silica microsphere material is added in mixed solution obtained by (4), under the conditions of 300 rpm of revolving speed
1h is stirred, makes its even suspension, so that the enhanced alkali-free quick-coagulant of nanosized seeds of the invention be made.
Embodiment 4
The preparation of the enhanced alkali-free quick-coagulant of nanosized seeds, comprising the following steps:
(1) the nano silica microsphere material is prepared.
(2) 37g aluminum sulfate, 5g magnesium sulfate are mixed with 30g distilled water, is stirred under 60 DEG C of water bath conditions to all molten
Solution, mixing speed 300rpm.
(3) it keeps temperature and speed of agitator constant, 10g triethanolamine is slowly added dropwise in the above solution, rate of addition is
1.0 ml/min。
(4) 3g salicylic acid is slowly added in above-mentioned mixed solution and is stirred, adjust mixed solution pH value to 3.0.
(5) 15g nano silica microsphere material is added in mixed solution obtained by (4), under the conditions of 300 rpm of revolving speed
1h is stirred, makes its even suspension, so that the enhanced alkali-free quick-coagulant of nanosized seeds of the invention be made.
Embodiment 5
The preparation of the enhanced alkali-free quick-coagulant of nanosized seeds, comprising the following steps:
(1) the nano silica microsphere material is prepared.
(2) 32g aluminum sulfate, 5g magnesium sulfate are mixed with 30g distilled water, is stirred under 60 DEG C of water bath conditions to all molten
Solution, mixing speed 300rpm.
(3) it keeps temperature and speed of agitator constant, 15g tetrahydroxyethyl-ethylene diamine is slowly added dropwise in the above solution, be added dropwise
Speed is 1.0 ml/min.
(4) 3g phosphoric acid is slowly added in above-mentioned mixed solution and is stirred, adjust mixed solution pH value to 3.0.
(5) 15g nano silica microsphere material is added in mixed solution obtained by (4), under the conditions of 300 rpm of revolving speed
1h is stirred, makes its even suspension, so that the enhanced alkali-free quick-coagulant of nanosized seeds of the invention be made.
Comparative example 1
40g aluminum sulfate, 8g magnesium sulfate are mixed with 36g distilled water, to whole dissolutions, stirring is fast for stirring under 60 DEG C of water bath conditions
Degree is 300rpm.5g tetrahydroxyethyl-ethylene diamine is slowly added dropwise, rate of addition is 1.0 ml/min.3g citric acid is slowly added to
It states in mixed solution and is stirred, adjust mixed solution pH value to 3.0.To obtain the alkali-free rapid hardening without nanosized seeds
Agent.
Comparative example 2
Comparison is prepared according to the proportion of embodiment 4 in Chinese patent CN1974466A " alkali-free liquid setting accelerator for spray concrete "
2 accelerator of example.
1 embodiment and comparative example the performance test results of table
| PERFORMANCE EXAMPLES | Volume/wt% | Presetting period/min:s | Final setting time/min:s | 1d compression strength/MPa | 28d intensity ratio/% | 90d strength retention ratio/% |
| Embodiment 1 | 7% | 2min58s | 8min32s | 12.35 | 101.1% | 101.0% |
| Embodiment 2 | 6% | 2min43s | 8min16s | 14.56 | 102.8% | 103.7% |
| Embodiment 3 | 5% | 2min16s | 7min58s | 16.56 | 105.6% | 107.1% |
| Embodiment 4 | 5% | 1min58s | 7min40s | 17.68 | 108.7% | 108.6% |
| Embodiment 5 | 5% | 1min45s | 7min25s | 19.53 | 114.4% | 111.8% |
| Comparative example 1 | 7% | 3min49s | 9min50s | 6.96 | 89.9% | 88.2% |
| Comparative example 2 | 7% | 4min5s | 10min31s | 6.56 | 83.8% | 81.0% |
Test result in upper table is obtained according to " gunite concrete accelerator " (GB ∕ T 35159-2017) test.By table 1
Known to: the content of nano silica seed crystal material described in 1 ~ embodiment of embodiment 4 is gradually increased.It can be bright from test result
It is aobvious to find out, compared with comparative example 1 is without the accelerator of nanosized seeds reinforcing material, with the raising of nanosized seeds content, each reality
The setting time for applying example gradually shortens, and each age glue sand test specimen compression strength significantly improves.Embodiment 4 and embodiment 5 are distinguished
In embodiment 5 is to further improve the usage amount of organic alcohol amine on the basis of the match ratio of embodiment 4.It can from experimental result
To find out, with the raising of organic alcohol amine usage amount, each age glue sand test piece intensity is also obviously improved.
Claims (2)
1. a kind of enhanced alkali-free quick-coagulant of nanosized seeds, which is characterized in that the alkali-free quick-coagulant includes the original of following mass parts
Material:
Lithium sulfate 0% ~ 15%；
Aluminum sulfate 30% ~ 50%；
Magnesium sulfate 5% ~ 10%；
Modified manometer silicon dioxide microballoon 5% ~ 15%；
Organic alcohol amine 5% ~ 15%；
Inorganic acid 3% ~ 5%；
Surplus is water,
The modified manometer silicon dioxide microballoon is the size as made from Electrostatic Absorption silica using polystyrene as matrix
For the particle of 50nm ~ 100nm, which serves as crystal seed in cement hydration process.
2. the enhanced alkali-free quick-coagulant of a kind of nanosized seeds according to claim 1, which is characterized in that preparation method
The following steps are included: step 1: with polystyrene spheres (PS) for matrix, adsorption cetyl trimethylammonium bromide (CTAB),
Using the electrostatic interaction of CTAB cation and ethyl orthosilicate (TEOS) hydrolysis silicon matter anion, the titanium dioxide that hydrolysis is obtained
Silicon is coated on PS ball, through filtering, cleaning and drying, the nano modification silicon dioxide microsphere is made, for use；
Step 2: lithium sulfate, aluminum sulfate and magnesium sulfate are mixed with water, temperature be 60 DEG C ~ 80 DEG C, speed of agitator be 300rpm ~
1h ~ 2h is reacted under conditions of 500 rpm；
Step 3: keeping temperature and speed of agitator constant, organic alcohol amine is slowly added dropwise, is at the uniform velocity added dropwise to complete in 0.5h ~ 1h；
Step 4: keeping temperature and speed of agitator constant, be slowly added to inorganic acid, adjust mixed liquor pH value to 2.0 ~ 4.0；
Step 5: being kept stirring that revolving speed is constant, the addition of modified manometer silicon dioxide microballoon made from step 1 step 4 is obtained mixed
It closes in liquid, stirs 0.5h ~ 1h, make its even suspension, be slowly cooled to room temperature, the enhanced alkali-free quick-coagulant of nanosized seeds is made.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113173727A (en) * | 2021-05-06 | 2021-07-27 | 中国铁路设计集团有限公司 | Novel environment-friendly liquid alkali-free cement accelerator |
| CN113698124A (en) * | 2021-09-14 | 2021-11-26 | 中铁十一局集团桥梁有限公司 | Alkali-free liquid accelerator and preparation method thereof |
| CN114180874A (en) * | 2021-12-31 | 2022-03-15 | 四川赢盛化工有限公司 | Additive composition agent of powder rapid repair material and application of additive composition agent in cement concrete |
| CN114804707A (en) * | 2022-05-11 | 2022-07-29 | 湖南腾达岩土工程技术有限公司 | Thixotropic agent for ultrahigh-performance sprayed concrete and preparation method and device thereof |
| CN114907070A (en) * | 2022-05-11 | 2022-08-16 | 湖南人健宝固高新科技发展有限公司 | Non-shrinkage sprayable ultrahigh-performance concrete and construction method thereof |
| CN116462441A (en) * | 2023-05-04 | 2023-07-21 | 湖北腾辰科技股份有限公司 | Early-strength fluorine-free alkali-free liquid accelerator and preparation method thereof |
| CN118666541A (en) * | 2024-08-23 | 2024-09-20 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Sulfate erosion resistant sprayed concrete preparation method, sprayed concrete and application |
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| CN114907070A (en) * | 2022-05-11 | 2022-08-16 | 湖南人健宝固高新科技发展有限公司 | Non-shrinkage sprayable ultrahigh-performance concrete and construction method thereof |
| CN116462441A (en) * | 2023-05-04 | 2023-07-21 | 湖北腾辰科技股份有限公司 | Early-strength fluorine-free alkali-free liquid accelerator and preparation method thereof |
| CN116462441B (en) * | 2023-05-04 | 2023-10-20 | 湖北腾辰科技股份有限公司 | Early-strength fluorine-free alkali-free liquid accelerator and preparation method thereof |
| CN118666541A (en) * | 2024-08-23 | 2024-09-20 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Sulfate erosion resistant sprayed concrete preparation method, sprayed concrete and application |
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