CN109265064A - A kind of preparation method of high-strength alkali-free chlorine-free accelerator - Google Patents
A kind of preparation method of high-strength alkali-free chlorine-free accelerator Download PDFInfo
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- CN109265064A CN109265064A CN201811138388.6A CN201811138388A CN109265064A CN 109265064 A CN109265064 A CN 109265064A CN 201811138388 A CN201811138388 A CN 201811138388A CN 109265064 A CN109265064 A CN 109265064A
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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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation methods of high-strength alkali-free chlorine-free accelerator: the following steps are included: it is 1) that 2- acrylamide-2-methyl propane sulfonic, acrylic acid, modified manometer silicon dioxide solution initiator and water ultrasonic disperse is uniform, 5-8h is reacted after being heated to 60-80 DEG C obtains mixed solution A；2) aluminum sulfate, hydramine, water and mixed solution A are heated to 60 ~ 80 DEG C of 1 ~ 5h of reaction, obtain mixed solution B；It is cooled to room temperature, then using mulser high speed dispersion 10 minutes to get high-strength alkali-free chlorine-free accelerator.This method can greatly improve the 1d compression strength of cement mortar, while the comprehensive performances such as stability that can promote product using organically-modified alkali-free chlorine-free accelerator obtained.
Description
Technical field
The invention belongs to technical field of concrete additives, in particular to a kind of preparation of high-strength alkali-free chlorine-free accelerator
Method.
Background technique
Accelerator is a kind of concrete admixture for making cement or concrete rapid condensation and hardening.Its main function is can
To increase coating thickness of gunite concrete, shorten the interval between secondary injection, while improving early strength of concrete, with
Supporting drag is just provided in time, has been widely used for modern underground engineering, mine engineering, leak stopping and the engineerings such as speedily carry out rescue work at present.
Alkali-free quick-coagulant just becomes the main side of accelerator development due to having little effect to late strength of concrete
To being since raw material sources are easy to get with aluminum sulfate alkali-free quick-coagulant as main component, preparation process is simple, is the master of accelerator
Want research object.Aluminum sulfate is not easy individually to be configured to alkali-free quick-coagulant, needs that other components is combined to solve stability and morning together
The problems such as strong.
Sodium aluminate, magnesium sulfate, calcium chloride, fluoride salt and silicate etc. are the common components of aluminum sulfate system alkali-free quick-coagulant,
If patent CN200610098296.0 discloses a kind of alkali-free liquid setting accelerator for spray concrete, rapid hardening is improved using magnesium sulfate
Agent improves the early strength of concrete, but the introducing of magnesium sulfate is easy to cause the crystallization of aluminum sulfate to the applicability of cement
It is precipitated, serious influence is caused on product stability.Hydrofluoric acid is also the usual ingredients of aluminum sulfate system alkali-free quick-coagulant, although hydrogen
Fluoric acid can significantly shorten setting time, improve the stability of product, but early strength is very low, cement mortar 1d pressure resistance
Degree is frequently less than 3MPa, is not able to satisfy the performance requirement of standard JC 477-2005 " gunite concrete accelerator ".
Summary of the invention
In order to solve the disadvantages of existing alkali-free quick-coagulant early strength is lower, the present invention provides a kind of high-strength alkali-free without
The preparation method of chlorine accelerator.
Nano silica can effectively facilitate hydrated cementitious, optimize interfacial structure, to improve cement-base composite material
Intensity.But nano silica is also a kind of thickener, if be added directly into alkali-free quick-coagulant, can greatly improve product
Viscosity, cause product solidification can not actually use.Furthermore nano silica is easy to reunite, directly since surface is rich in hydroxyl
It is very low to connect modification by copolymerization grafting rate.
The preparation method of strong type alkali-free chlorine-free accelerator of the present invention, comprising the following steps:
Step (1) divides 2- acrylamide-2-methyl propane sulfonic, acrylic acid, modified manometer silicon dioxide, initiator and water ultrasound
It dissipates and mixes, 5-8h is reacted after being heated to 60-80 DEG C and obtains mixed solution A；
Aluminum sulfate, hydramine, water and mixed solution A are heated to 60-80 DEG C of reaction 1-5h by step (2), obtain mixed solution B；Drop
It warms to room temperature, then using mulser high speed dispersion 10 minutes to get high-strength alkali-free chlorine-free accelerator.
Further improvement of the present invention, mixed solution A described in step (1) are made of by mass percentage following components:
2- acrylamide-2-methyl propane sulfonic 10-15%
Acrylic acid 1-5%
Modified manometer silicon dioxide 20-30%
Initiator 0.1-1%
Water surplus
The initiator is ammonium persulfate and sodium hydrogensulfite, and wherein the molar ratio of ammonium persulfate and sodium hydrogensulfite is 2-5:1.
Further improvement of the present invention, mixed solution B described in step (2) are made of by mass percentage following components:
Aluminum sulfate 40-60%
Hydramine 2-12%
Mixed solution A 6-12%
Water surplus
The linear velocity of the dispersion of mulser described in step (2) is 20-30m/s, and the heating temperature is 50-80 DEG C.
Further improvement of the present invention, the hydramine are one of diethanol amine or triethanolamine.
In the present invention, the modified manometer silicon dioxide preparation method the following steps are included:
(1) nano silica after being dried in vacuo 2g is added in 40ml N-Methyl pyrrolidone, then with Ultrasound Instrument point
1h is dissipated, evenly dispersed suspension is obtained；
(2) 4g γ-methacryloxypropyl trimethoxy silane is added in 40ml N-Methyl pyrrolidone, is stirred
Uniformly, it is added in three batches in the suspension of step (1)；
(3) above-mentioned mixed solution is transferred in the flask under nitrogen protection, is stirred to react for 24 hours at a temperature of 80 DEG C, then from
The heart separates, and vacuum drying obtains modified manometer silicon dioxide at ethanol washing 5 times, last 60 DEG C.
Above-mentioned high-strength alkali-free chlorine-free accelerator of stating is in gunite concrete field, volume to be the 6- of cement consumption
10wt%。
Beneficial effects of the present invention: alkali-free quick-coagulant is modified by nanometer titanium dioxide silicon polymer, can be improved
Cement granules and the direct compatibility of polymer and adhesion strength, the alkali-free quick-coagulant containing nano silica can be with simultaneously
The combination gap between hydrated product C-S-H gel is filled, improves the interface microstructure of cement and aggregate, to promote product
1d compression strength.
Specific embodiment
In order to deepen the understanding to this method, this method is described in further detail below in conjunction with embodiment, the reality
It applies example to be only used for explaining this method, the protection scope of this method is not constituted and limited.
For a better understanding of the present invention, the contents of the present invention are further described below with reference to embodiment, but this
The content of invention is not limited to the scope of the embodiments.
Modified manometer silicon dioxide is prepared first:
(1) nano silica after being dried in vacuo 2g is added in 40ml N-Methyl pyrrolidone, then with Ultrasound Instrument point
1h is dissipated, evenly dispersed suspension is obtained；
(2) 4g γ-methacryloxypropyl trimethoxy silane is added in 40ml N-Methyl pyrrolidone, is stirred
Uniformly, it is added in three batches in the suspension of step (1)；
(3) above-mentioned mixed solution is transferred in the flask under nitrogen protection, is stirred to react for 24 hours at a temperature of 80 DEG C, then from
The heart separates, and vacuum drying obtains modified manometer silicon dioxide at ethanol washing 5 times, last 60 DEG C.
Embodiment 1
The preparation of high-strength alkali-free chlorine-free accelerator, comprising the following steps:
(1) by 10g 2- acrylamide -2- methacrylic acid, 1g acrylic acid, 20g nano silica, 0.92g ammonium persulfate,
0.08g sodium hydrogensulfite and the mixing of 68.9g water, react 8 hours after being heated to 80 DEG C and obtain mixed solution A；
(2) 60g aluminum sulfate, 12g diethanol amine, 12g mixed solution A and 16g water are heated to 80 DEG C of reaction 5h, obtain mixing molten
Liquid B；Be cooled to room temperature, then use emulsifier high speed dispersion 10 minutes, the linear velocity of dispersion be 20m/s to get high-strength without
Alkali is without chlorine accelerator.
Embodiment 2
The preparation of high-strength alkali-free chlorine-free accelerator, comprising the following steps:
(1) by 12g 2- acrylamide -2- methacrylic acid, 2g acrylic acid, 20g nano silica, 0.92g ammonium persulfate,
0.08g sodium hydrogensulfite and the mixing of 65g water, react 5 hours after being heated to 60 DEG C and obtain mixed solution A；
(2) 40g aluminum sulfate, 2g diethanol amine, 6g mixed solution A and 52g water are heated to 50 DEG C of reaction 1h, obtain mixed solution
B；It is cooled to room temperature, is then used emulsifier high speed dispersion 10 minutes, the linear velocity of dispersion is 30m/s to get high-strength alkali-free
Without chlorine accelerator.
Embodiment 3
The preparation of high-strength alkali-free chlorine-free accelerator, comprising the following steps:
(1) by 15g 2- acrylamide -2- methacrylic acid, 5g acrylic acid, 30g nano silica, 0.08g ammonium persulfate,
0.02g sodium hydrogensulfite and the mixing of 49.9g water, react 5 hours after being heated to 60 DEG C and obtain mixed solution A；
(2) 50g aluminum sulfate, 10g triethanolamine, 8g mixed solution A and 32g water are heated to 50 DEG C of reaction 2h, obtain mixing molten
Liquid B；Be cooled to room temperature, then use emulsifier high speed dispersion 10 minutes, the linear velocity of dispersion be 25m/s to get high-strength without
Alkali is without chlorine accelerator.
Embodiment 4
The preparation of high-strength alkali-free chlorine-free accelerator, comprising the following steps:
(1) by 14g 2- acrylamide -2- methacrylic acid, 5g acrylic acid, 25g nano silica, 0.08g ammonium persulfate,
0.02g sodium hydrogensulfite and the mixing of 55.9g water, react 7 hours after being heated to 70 DEG C and obtain mixed solution A；
(2) 50g aluminum sulfate, 10g diethanol amine, 8g mixed solution A and 32g water are heated to 60 DEG C of reaction 3h, obtain mixing molten
Liquid B；Be cooled to room temperature, then use emulsifier high speed dispersion 10 minutes, the linear velocity of dispersion be 20m/s to get high-strength without
Alkali is without chlorine accelerator.
Comparative example 1
60g aluminum sulfate, 12g diethanol amine and 28g water are heated to 80 DEG C of reaction 5h, obtain alkali-free quick-coagulant.
Comparative example 2
The nano silica that 2.4wt% is added on the basis of comparative example 1 prepares alkali-free quick-coagulant.
Comparative example 3
The modified manometer silicon dioxide that 2.4wt% is added on the basis of comparative example 1 prepares alkali-free quick-coagulant.
The performance of alkali-free quick-coagulant made from testing example 1 to 4 and comparative example 1 to 3, the results are shown in Table 1.
Test is with the test method of material, setting time and compression strength referring to Chinese building material professional standard JC477-
2005.Cement used is 42.5 cement of P.O of Jiangsu He Lin Cement Co., Ltd production.
Layered values: weighing 100ml alkali-free quick-coagulant into 100ml graduated cylinder, stands after a week, visual observations stablize disposition
Condition, the supernatant volume value occurred in graduated cylinder are layered values.
Viscosity number: weighing 100ml alkali-free quick-coagulant, stands after a week, flies viscosimeter test using rich strangle of Brookfield
Its viscosity number.If fruit product is layered, its viscosity is surveyed again after mixing evenly.
1 embodiment and comparative example the performance test results of table
| Performance Embodiment | Volume/ wt% | Presetting period/ Min:s | Final setting time/ Min:s | 1d pressure resistance Degree/MPa | 28d pressure resistance Degree/MPa | Layering Value/ml | Viscosity Value/cp |
| Embodiment 1 | 8 | 3:10 | 7:00 | 18 | 57 | 0 | 115 |
| Embodiment 2 | 8 | 3:30 | 7:13 | 17 | 53 | 1 | 120 |
| Embodiment 3 | 8 | 3:00 | 7:05 | 18 | 55 | 0 | 116 |
| Embodiment 4 | 8 | 3:05 | 8:00 | 16 | 51 | 0 | 127 |
| Comparative example 1 | 8 | 5:00 | 11:00 | 7.8 | 48 | 65 | 132 |
| Comparative example 2 | 3 | 4:30 | 11:30 | 14 | 56 | 0 | Solidification |
| Comparative example 3 | 8 | 4:52 | 10:50 | 17 | 51 | 50 | 1603 |
Seen from table 1: the alkali-free quick-coagulant performance combined only with hydramine and aluminum sulfate is bad, is not able to satisfy JC477-2005 mark
Quasi- performance requirement.1d compression strength can be significantly improved later by introducing nano silica, but due to nano silica
Has the effect of thickening, therefore solidification phenomenon occurs after a week in the alkali-free quick-coagulant placement prepared, can not pour out from graduated cylinder, nothing
Method meets the field demand of actual ejection concrete.Although modified manometer silicon dioxide significantly reduces the viscous of alkali-free quick-coagulant
Degree, but still have the viscosity number of 1603cp.It is provided by the invention by nanometer titanium dioxide silicon polymer to alkali-free quick-coagulant into
Row is modified, and cement granules and the direct compatibility of polymer and adhesion strength can be improved, simultaneously containing nano silica
Alkali-free quick-coagulant can also fill the combination gap between hydrated product C-S-H gel, improve the micro- knot in interface of cement and aggregate
Structure, to promote the 1d compression strength of product.
The basic principles and main features and advantage of this method have been shown and described above.The technical staff of the industry should
Understand, this method is not restricted to the described embodiments, and the above embodiments and description only describe the originals of this method
Reason, under the premise of not departing from this method spirit and scope, this method be will also have various changes and improvements, these changes and improvements
It both falls within the scope of claimed this method.Process require that protection scope is by appended claims and its equivalent circle
It is fixed.
Claims (7)
1. a kind of preparation method of high-strength alkali-free chlorine-free accelerator, which comprises the following steps:
Step (1) divides 2- acrylamide-2-methyl propane sulfonic, acrylic acid, modified manometer silicon dioxide, initiator and water ultrasound
It dissipates and mixes, 5-8h is reacted after being heated to 60-80 DEG C and obtains mixed solution A；
Aluminum sulfate, hydramine, water and mixed solution A are heated to 60-80 DEG C of reaction 1-5h by step (2), obtain mixed solution B；Drop
It warms to room temperature, then using mulser high speed dispersion 10 minutes to get high-strength alkali-free chlorine-free accelerator.
2. the preparation method of high-strength alkali-free chlorine-free accelerator according to claim 1, which is characterized in that in step (1)
The mixed solution A is made of by mass percentage following components:
2- acrylamide-2-methyl propane sulfonic 10-15%
Acrylic acid 1-5%
Modified manometer silicon dioxide 20-30%
Initiator 0.1-1%
Water surplus
The initiator is ammonium persulfate and sodium hydrogensulfite, and wherein the molar ratio of ammonium persulfate and sodium hydrogensulfite is 2-5:1.
3. the preparation method of high-strength alkali-free chlorine-free accelerator according to claim 1, which is characterized in that in step (2)
The mixed solution B is made of by mass percentage following components:
Aluminum sulfate 40-60%
Hydramine 2-12%
Mixed solution A 6-12%
Water surplus.
4. the preparation method of high-strength alkali-free chlorine-free accelerator according to claim 1, which is characterized in that in step (2)
The linear velocity of the mulser dispersion is 20-30m/s, and heating temperature is 50-80 DEG C.
5. the preparation method of high-strength alkali-free chlorine-free accelerator according to claim 1, it is characterised in that the hydramine is
One of diethanol amine or triethanolamine.
6. the preparation method of high-strength alkali-free chlorine-free accelerator according to claim 2, which is characterized in that the modification is received
Rice silica preparation method the following steps are included:
(1) nano silica after being dried in vacuo 2g is added in 40ml N-Methyl pyrrolidone, then with Ultrasound Instrument point
1h is dissipated, evenly dispersed suspension is obtained；
(2) 4g γ-methacryloxypropyl trimethoxy silane is added in 40ml N-Methyl pyrrolidone, is stirred
Uniformly, it is added in three batches in the suspension of step (1)；
(3) above-mentioned mixed solution is transferred in the flask under nitrogen protection, is stirred to react for 24 hours at a temperature of 80 DEG C, then from
The heart separates, and vacuum drying obtains modified manometer silicon dioxide at ethanol washing 5 times, last 60 DEG C.
7. high-strength alkali-free chlorine-free accelerator described in any one of claim 1-5, which is characterized in that the high-strength alkali-free
No chlorine accelerator is in gunite concrete field, volume to be the 6-10wt% of cement consumption.
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| CN110606695A (en) * | 2019-10-17 | 2019-12-24 | 江苏兆佳建材科技有限公司 | Modified polycarboxylate superplasticizer and preparation method thereof |
| CN110981266A (en) * | 2019-11-27 | 2020-04-10 | 江苏苏博特新材料股份有限公司 | Special anti-settling agent for alkali-free accelerator, and preparation method and application thereof |
| CN111646728A (en) * | 2020-07-01 | 2020-09-11 | 中建材中岩科技有限公司 | Quick-setting high-strength alkali-free liquid accelerator |
| CN112723787A (en) * | 2020-12-30 | 2021-04-30 | 山西佳维新材料股份有限公司 | Fluorine-free liquid accelerator and preparation method and application thereof |
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