CN109293269A - A kind of preparation method of early-strength alkali-free liquid accelerator - Google Patents
A kind of preparation method of early-strength alkali-free liquid accelerator Download PDFInfo
- Publication number
- CN109293269A CN109293269A CN201811492517.1A CN201811492517A CN109293269A CN 109293269 A CN109293269 A CN 109293269A CN 201811492517 A CN201811492517 A CN 201811492517A CN 109293269 A CN109293269 A CN 109293269A
- Authority
- CN
- China
- Prior art keywords
- early
- free liquid
- preparation
- liquid accelerator
- alkali
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of early-strength alkali-free liquid accelerator, belong to building material technical field.Accelerator of the present invention is prepared by the component of following mass percentage: aluminum sulfate 55%-70%, magnesium sulfate 5%-10%, modified hydramine 5%-10%, organic acid 2%-5%, stabilizer 1%-3%, EDTA1%-3%, calcium formate 0.5%-2%, remaining is water.Specifically comprise the following steps: the preparation of (1) modified hydramine；(2): the preparation of early-strength alkali-free liquid accelerator.Early-strength alkali-free liquid accelerator prepared by the present invention can be used in gunite concrete industry, its alkali content is less than 1%, stationary phase was more than 3 months, 1d compression strength can achieve 19.93MPa, 28d compression strength loss is small, it is a kind of early-strength alkali-free liquid accelerator, can be widely applied to the initial construction and repairing of various architectural engineerings.
Description
Technical field
The invention belongs to building material technical fields, and in particular to a kind of early-strength alkali-free liquid accelerator and its preparation side
Method.
Background technique
Accelerator refers to the additive for hardening, its rapid condensation in cement concrete.China was from 90 years 20th century
In generation, starts to promote concrete spraying construction technology, guarantees that injection final product quality and reasonable construction process become critical issue.It develops
The good accelerator of the solidifying effect of function admirable, rush is its premise guarantee out.
Currently, accelerator is divided into powder and two kinds of liquid, and powder accelerator therein, because the operating condition of construction is poor, and
Construction personnel's health is damaged, work progress should not control, and just gradually be substituted by liquid accelerator.And liquid accelerator is nowadays
It mainly include low alkali, alkali-free two major classes in field application.Low alkali accelerator main component is NaAlO2、NaSiO4And combination product；
Alkali-free liquid accelerator main component is Al2(SO4)3And combination product.Traditional aluminate low-alkali liquid quick-setting agent component list
One, main by promoting the aquation of aluminium mineral material in cement to make cement rapid condensation, the cement more for mineral admixture
Adaptability it is poor.
In addition, from the point of view of presently disclosed related patents, though the entitled alkali-free quick-coagulant of partial monopoly, its be formulated in introduce
Alkali often beyond 1%, such as Shanxi can rise environmentally friendly Science and Technology Co., Ltd.'s invention disclosed patent (application number:
2016108141346), though alkali content reaches as high as 11.1% in entitled alkali-free quick-coagulant reality formula；Shanxi Hua Kai great achievement
Science and Technology Ltd.'s invention disclosed patent (application number: 2017101015775) entitled alkali-free quick-coagulant but actually alkali in formula
Content reaches as high as 13.3%.The higher one side of alkali content causes corrosion to injure construction personnel in concrete accelerator, damage
On the other hand human health may also cause alkali-aggregate reaction in concrete, late strength of concrete and durability is caused to decline.It is long
Pacifying university's invention disclosed patent, (application number: the accelerator early strength 2016110965096) provided is lower, is easy to influence spray
Penetrate concrete normal construction.In conclusion the alkali-free liquid accelerator tool developing a kind of real alkali-free and haveing excellent performance
There is important meaning.
Summary of the invention
The present invention is aided with modified hydramine organic micromolecule and EDTA conduct based on aluminum sulfate alkali-free liquid accelerator
Complexant promotes aluminium ion in conjunction with the coordination of functional group, enhances its stability in highly concentrated solution.It is aided with formic acid simultaneously
Calcium makes up the accelerator disadvantage not high due to getting up early intensity caused by rapid condensation, a kind of obtained early-strength haveing excellent performance without
Alkali liquid quick-setting agent and preparation method thereof.The accelerator can guarantee early strength qualification while shortening the rapid hardening time, and
Adaptability is good, prepares simple, practical, energy saving.The purpose to realize the present invention, used technical solution is:
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst is added according to molar ratio 1:2-3:0.0034-0.01 in mouth bottle, is reacted at 65-90 DEG C
After 1-2.5h, 2-3mol organic acid reaction 0.5-1h is added in obtained mixed solution, obtains modified hydramine；
(2) aluminum sulfate, magnesium sulfate and organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three-necked flask
In, deionized water is added, 1-2h is stirred with 300r/min-400r/min under 60 DEG C of -90 DEG C of waters bath with thermostatic control, obtains accelerator mother
Liquid；It under 60 DEG C of -75 DEG C of waters bath with thermostatic control, is stirred with 300r/min-400r/min, step (1) institute is added into accelerator mother liquor
Hydramine must be modified, continue to stir 30min, add calcium formate, stir 30min, after EDTA is added, at 65 DEG C -70 DEG C
Insulated and stirred 40min is added stabilizer, then stirs 20min with 200r/min-300r/min after being cooled to room temperature, obtain the morning
Strong type alkali-free liquid accelerator.
Hydramine described in step (1) is monoethanolamine, diethanol amine, triethanolamine, triisopropanolamine, diethanol list isopropyl
One or more of hydramine.
Amine organic matter described in step (1) be ethylenediamine, p-phenylenediamine, Putriscine, new pentanediamine, decamethylene diamine or
One or more of 2 methyl pentamethylenediamine.
Step (1) catalyst is one of p-methyl benzenesulfonic acid, anhydrous sodium acetate, aluminium chloride or zinc chloride or several
Kind.
The organic acid is one or more of oxalic acid, propionic acid, salicylic acid or benzoic acid.
The stabilizer is one or more of citric acid, glycine, alanine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator as prepared by the above method, is made of the raw material of following mass fraction
: aluminum sulfate 55%-70%, magnesium sulfate 5%-10%, modified hydramine 5%-10%, organic acid 2%-5%, stabilizer 1%-
3%, EDTA1%-3%, calcium formate 0.5%-2%, remaining is deionized water.
The aluminum sulfate that the present invention uses is mixed with magnesium sulfate as accelerator bulk composition, wherein the magnesium ion introduced is in water
During muddy water, OH can be preferentially combined-It is formed Mg (OH)2As solidifying nuclear particle, accelerate hydrated cementitious process.High-content aluminium from
Chemistry imbalance caused by son leads to gypsum and C3A is more easier to dissolve, and promotes the generation of early stage a large amount of entringite, to reach
The effect of rapid hardening.Calcium formate and modified hydramine can effectively improve the solidifying and early epistasis energy of rush of accelerator in the present invention.
Compared with prior art, the invention has the following advantages: (1) alkali-free liquid accelerator provided by the invention is pressed
More solito is added in jet cement composition, and the early strength of concrete rapidly develops, and does not influence later strength, gram
A large amount of incorporations of conventional alkaline accelerator have been taken so that the drawbacks of late strength of concrete is decreased obviously；(2) provided by the invention
Alkali-free liquid accelerator substantially reduces a possibility that generating alkali-aggregate reaction；(3) alkali-free quick-coagulant and cement provided by the invention
Adaptability it is good, the requirement of construction of shotcrete is all satisfied to the cement of different brands.
Specific embodiment
Technical scheme is described further combined with specific embodiments below, but not limited to this.
Embodiment 1
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:3:0.005, after 65 DEG C of reaction 1h, what is obtained is added in mouth bottle
2mol organic acid reaction 0.5h is added in mixed solution, obtains modified hydramine；
(2) 60g aluminum sulfate, 6g magnesium sulfate and 6g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 30g deionized water is added, 1.5h is stirred with 400r/min under 80 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；?
It under 65 DEG C of waters bath with thermostatic control, is stirred with 350r/min, then modified hydramine 6g obtained by step (1) is added into accelerator mother liquor, continued
Stir 30min, add 1.5g calcium formate, stir 30min, after 2gEDTA is added, the insulated and stirred 40min at 65 DEG C,
2g stabilizer is added after being cooled to room temperature, then 20min is stirred with 300r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is diethanol amine.
Amine organic matter described in step (1) is ethylenediamine.
Step (1) catalyst is p-methyl benzenesulfonic acid.
The organic acid is oxalic acid.
The stabilizer is citric acid.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 55%, sulfuric acid
Magnesium 5%, modified hydramine 5%, organic acid 2%, stabilizer 1%, EDTA1%, calcium formate 1%, remaining is deionized water.
Embodiment 2
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:2.5:0.0045 is added in mouth bottle.After 65 DEG C of reaction 1.5h,
3mol organic acid reaction 45min is added in obtained mixed solution, obtains modified hydramine；
(2) 75g aluminum sulfate, 8g magnesium sulfate and 5g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 19g deionized water is added, 2h is stirred with 400r/min under 80 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；65
It under DEG C water bath with thermostatic control, is stirred with 400r/min, then modified hydramine 10g obtained by step (1) is added into accelerator mother liquor, continue to stir
Mix 30min, add 2g calcium formate, stir 30min, after 2.5gEDTA is added, insulated and stirred 40min, cold at 65 DEG C
But to 3g stabilizer is added after room temperature, then 20min stirred with 300r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is triisopropanolamine.
Amine organic matter described in step (1) is ethylenediamine.
Step (1) catalyst is p-methyl benzenesulfonic acid.
The organic acid is oxalic acid.
The stabilizer is citric acid.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 60%, sulfuric acid
Magnesium 6%, modified hydramine 8%, organic acid 4%, stabilizer 2%, EDTA2%, calcium formate 1%, remaining is deionized water.
Embodiment 3
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:3:0.01 is added in mouth bottle.After 75 DEG C of reaction 1h, what is obtained
3mol organic acid reaction 45min is added in mixed solution, obtains modified hydramine；
(2) 85g aluminum sulfate, 10g magnesium sulfate and 5g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 20g deionized water is added, 2h is stirred with 400r/min under 85 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；70
It under DEG C water bath with thermostatic control, is stirred with 400r/min, then modified hydramine 10g obtained by step (1) is added into accelerator mother liquor, continue to stir
Mix 30min, add 3g calcium formate, stir 30min, after 3gEDTA is added, the insulated and stirred 40min at 65 DEG C is cooling
5g stabilizer is added after to room temperature, then 20min is stirred with 300r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is triethanolamine.
Amine organic matter described in step (1) is Putriscine.
Step (1) catalyst is anhydrous sodium acetate.
The organic acid is benzoic acid.
The stabilizer is glycine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 60%, sulfuric acid
Magnesium 7%, modified hydramine 7%, organic acid 3%, stabilizer 3%, EDTA2%, calcium formate 2%, remaining is deionized water.
Embodiment 4
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:2:0.01 is added in mouth bottle.After 80 DEG C of reaction 2h, what is obtained
2.5mol organic acid reaction 45min is added in mixed solution, obtains modified hydramine；
(2) 78g aluminum sulfate, 6g magnesium sulfate and 5g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 19g deionized water is added, 2h is stirred with 400r/min under 85 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；70
It under DEG C water bath with thermostatic control, is stirred with 400r/min, then modified hydramine 8g obtained by step (1) is added into accelerator mother liquor, continue to stir
Mix 30min, add calcium formate 0.5g, stir 30min, after EDTA1.5g is added, the insulated and stirred 40min at 65 DEG C,
Stabilizer 3g is added after being cooled to room temperature, then 20min is stirred with 300r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is triethanolamine.
Amine organic matter described in step (1) is p-phenylenediamine.
Step (1) catalyst is anhydrous sodium acetate.
The organic acid is salicylic acid.
The stabilizer is glycine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 64%, sulfuric acid
Magnesium 5%, modified hydramine 6%, organic acid 4%, stabilizer 2%, EDTA1%, calcium formate 0.5%, remaining is deionized water.
Embodiment 5
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:2:0.0035 is added in mouth bottle.After 72 DEG C of reaction 1h, obtaining
Mixed solution 2.5mol organic acid reaction 1h is added, obtain modified hydramine；
(2) 90g aluminum sulfate, 10g magnesium sulfate and 6g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 10g deionized water is added, 1.5h is stirred with 400r/min under 85 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；?
It under 65 DEG C of waters bath with thermostatic control, is stirred with 400r/min, then modified hydramine 8g obtained by step (1) is added into accelerator mother liquor, continued
Stir 30min, add calcium formate 2.5g, stir 30min, after EDTA4g is added, the insulated and stirred at 65 DEG C DEG C
40min is added stabilizer 4g, then stirs 20min with 300r/min after being cooled to room temperature, obtain the early-strength alkali-free liquid rapid hardening
Agent.
Hydramine described in step (1) is diethanol monoisopropanolamine.
Amine organic matter described in step (1) is decamethylene diamine.
Step (1) catalyst is aluminium chloride.
The organic acid is oxalic acid.
The stabilizer is alanine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 67%, sulfuric acid
Magnesium 7%, modified hydramine 6%, organic acid 5%, stabilizer 3%, EDTA3%, calcium formate 2%, remaining is deionized water.
Embodiment 6
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:3:0.003 is added in mouth bottle.After 80 DEG C of reaction 15h, obtaining
Mixed solution 2.5mol organic acid reaction 1h is added, obtain modified hydramine；
(2) 80g aluminum sulfate, 8g magnesium sulfate and 5g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 20g deionized water is added, 2h is stirred with 400r/min under 85 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；65
It under DEG C water bath with thermostatic control, is stirred with 400r/min, then modified hydramine 8g obtained by step (1) is added into accelerator mother liquor, continue to stir
Mix 30min, add calcium formate 2g, stir 30min, after EDTA3g is added, the insulated and stirred 40min at 65 DEG C is cooling
Stabilizer 3g is added after to room temperature, then 20min is stirred with 300r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is diethanol amine.
Amine organic matter described in step (1) is 2 methyl pentamethylenediamine.
Step (1) catalyst is zinc chloride.
The organic acid is benzoic acid.
The stabilizer is alanine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 62%, sulfuric acid
Magnesium 6%, modified hydramine 6%, organic acid 4%, stabilizer 2%, EDTA2%, calcium formate 1%, remaining is deionized water.
Embodiment 7
A kind of preparation method of early-strength alkali-free liquid accelerator, comprising the following steps:
(1) preparation method of modified hydramine: in the 250ml tetra- that mechanical stirring device, circulation condensation device, thermometer are housed
Hydramine, amine organic matter and catalyst, molar ratio 1:2.5:0.0034 is added in mouth bottle.After 90 DEG C of reaction 2h,
2mol organic acid reaction 0.5-1h is added in the mixed solution arrived, obtains modified hydramine；
(2) 90g aluminum sulfate, 10g magnesium sulfate and 5g organic acid first the preparation of early-strength alkali-free liquid accelerator: are placed in three
In mouth flask, 6g deionized water is added, 2h is stirred with 300r/min under 90 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；75
It under DEG C water bath with thermostatic control, is stirred with 300r/min, then modified hydramine 10g obtained by step (1) is added into accelerator mother liquor, continue to stir
Mix 30min, add calcium formate 2g, stir 30min, after EDTA3g is added, the insulated and stirred 40min at 70 DEG C is cooling
Stabilizer 3g is added after to room temperature, then 20min is stirred with 200r/min, obtains the early-strength alkali-free liquid accelerator.
Hydramine described in step (1) is triethanolamine.
Amine organic matter described in step (1) is 2 methyl pentamethylenediamine.
Step (1) catalyst is zinc chloride.
The organic acid is benzoic acid.
The stabilizer is glycine.
The aluminum sulfate is technical grade, wherein mass fraction >=16.00% of aluminium oxide.
The magnesium sulfate is technical grade, purity >=98%.
The calcium formate is to analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
A kind of early-strength alkali-free liquid accelerator is made of the raw material of following mass fraction: aluminum sulfate 70%, sulfuric acid
Magnesium 7%, modified hydramine 7%, organic acid 3%, stabilizer 2%, EDTA2%, calcium formate 1%, remaining is deionized water.
Test case
Cement paste setting time and cement mortar strength test:
The liquid accelerator that embodiment 1-7 is obtained is added in cement slurry according to the 4% of cement weight and 6%.According to
The requirement of Chinese building material professional standard JC477-2005 " gunite concrete accelerator " carries out cement paste setting time and water
Earth rubber sand strength test.Test result is shown in Table 1.
1 cement paste setting time of table and cement mortar strength test
The rapid hardening effect that can be seen that prepared liquid accelerator from the data in table 1 is obvious, greatly shortens solidifying
The time is tied, and the intensity of 1d is higher, the loss of strength of 28d is small, needed for fully meeting scene, has reached desired effect.
It should be noted that above-described embodiment is only the section Example for realizing preferred embodiment of the invention, Er Feiquan
Portion's embodiment.Obviously, it is based on the above embodiment of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of other all embodiments obtained, should fall within the scope of the present invention.
Claims (10)
1. a kind of preparation method of early-strength alkali-free liquid accelerator, which comprises the following steps:
(1) preparation method of modified hydramine: in the 250ml four-hole bottle that mechanical stirring device, circulation condensation device, thermometer are housed
According to molar ratio 1:2-3:0.0034-0.01 hydramine, amine organic matter and catalyst is added, in 65-90 DEG C of reaction 1-
After 2.5h, 2-3mol organic acid reaction 0.5-1h is added in obtained mixed solution, obtains modified hydramine；
(2) preparation of early-strength alkali-free liquid accelerator: being placed in three-necked flask by by aluminum sulfate, magnesium sulfate and organic acid, then
Deionized water is added, 1-2h is stirred with 300r/min-400r/min under 60 DEG C of -90 DEG C of waters bath with thermostatic control, obtains accelerator mother liquor；?
It under 60 DEG C of -75 DEG C of waters bath with thermostatic control, is stirred with 300r/min-400r/min, then is added into accelerator mother liquor and changes obtained by step (1)
Property hydramine, continue to stir 30min, add calcium formate, stir 30min, after EDTA is added, kept the temperature at 65 DEG C -70 DEG C
40min is stirred, stabilizer is added after being cooled to room temperature, then 20min is stirred with 200r/min-300r/min, obtains the early-strength
Alkali-free liquid accelerator.
2. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that institute in step (1)
Stating hydramine is one or more of monoethanolamine, diethanol amine, triethanolamine, triisopropanolamine, diethanol monoisopropanolamine.
3. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that institute in step (1)
Stating amine organic matter is one in ethylenediamine, p-phenylenediamine, Putriscine, new pentanediamine, decamethylene diamine or 2 methyl pentamethylenediamine
Kind is several.
4. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that step (1) is described
Catalyst is one or more of p-methyl benzenesulfonic acid, anhydrous sodium acetate, aluminium chloride or zinc chloride.
5. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that the organic acid is
One or more of oxalic acid, propionic acid, salicylic acid or benzoic acid.
6. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that the stabilizer is
One or more of citric acid, glycine, alanine.
7. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that the aluminum sulfate is
Technical grade, wherein mass fraction >=16.00% of aluminium oxide.
8. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that the magnesium sulfate is
Technical grade, purity >=98%.
9. the preparation method of early-strength alkali-free liquid accelerator according to claim 1, which is characterized in that the calcium formate is
Analyze pure, purity >=99.5%；The EDTA is to analyze pure, purity >=99.5%.
10. speed prepared by a kind of preparation method of the early-strength alkali-free liquid accelerator as described in claim 1-9 any one
Solidifying agent, which is characterized in that be made of the raw material of following mass fraction: aluminum sulfate 55%-70%, magnesium sulfate 5%-10%,
Modified hydramine 5%-10%, organic acid 2%-5%, stabilizer 1%-3%, EDTA1%-3%, calcium formate 0.5%-2%, remaining
For deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811492517.1A CN109293269B (en) | 2018-12-07 | 2018-12-07 | Preparation method of early-strength alkali-free liquid accelerator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811492517.1A CN109293269B (en) | 2018-12-07 | 2018-12-07 | Preparation method of early-strength alkali-free liquid accelerator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109293269A true CN109293269A (en) | 2019-02-01 |
| CN109293269B CN109293269B (en) | 2021-03-02 |
Family
ID=65142700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811492517.1A Active CN109293269B (en) | 2018-12-07 | 2018-12-07 | Preparation method of early-strength alkali-free liquid accelerator |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109293269B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748533A (en) * | 2019-03-04 | 2019-05-14 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | A kind of core master batch and preparation method thereof for alkali-free liquid setting accelerator |
| CN110330255A (en) * | 2019-07-02 | 2019-10-15 | 安徽海螺新材料科技有限公司 | It is a kind of to promote solidifying type liquid grinding aid and preparation method thereof |
| CN113087441A (en) * | 2021-03-05 | 2021-07-09 | 山西佳维新材料股份有限公司 | Fluoride-free liquid alkali-free accelerator and preparation method and application thereof |
| CN113480226A (en) * | 2021-08-02 | 2021-10-08 | 江西立晶新材料科技有限公司 | Liquid alkali-free accelerator and preparation method and application thereof |
| CN116283024A (en) * | 2023-03-21 | 2023-06-23 | 安宁市云洲新型建材有限公司 | Environment-friendly liquid alkali-free accelerator and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923988A (en) * | 2012-11-29 | 2013-02-13 | 北京冶建特种材料有限公司 | Liquid alkali-free chloride-free accelerating agent as well as methods for preparing and using same |
| JP2014152058A (en) * | 2013-02-06 | 2014-08-25 | Denki Kagaku Kogyo Kk | Liquid quick setting agent, cement composition using the same, and spraying method |
| CN105174796A (en) * | 2015-10-16 | 2015-12-23 | 杨洋 | Alkali-free liquid concrete setting accelerator and preparation method thereof |
| CN105776939A (en) * | 2016-03-15 | 2016-07-20 | 江苏中铁奥莱特新材料有限公司 | Preparation method for reinforced low-resilience and low-alkaline liquid concrete accelerator |
| CN107572856A (en) * | 2017-10-09 | 2018-01-12 | 常州琨瑶纺织品有限公司 | A kind of green alkali-free liquid concrete accelerator and preparation method thereof |
-
2018
- 2018-12-07 CN CN201811492517.1A patent/CN109293269B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923988A (en) * | 2012-11-29 | 2013-02-13 | 北京冶建特种材料有限公司 | Liquid alkali-free chloride-free accelerating agent as well as methods for preparing and using same |
| JP2014152058A (en) * | 2013-02-06 | 2014-08-25 | Denki Kagaku Kogyo Kk | Liquid quick setting agent, cement composition using the same, and spraying method |
| CN105174796A (en) * | 2015-10-16 | 2015-12-23 | 杨洋 | Alkali-free liquid concrete setting accelerator and preparation method thereof |
| CN105776939A (en) * | 2016-03-15 | 2016-07-20 | 江苏中铁奥莱特新材料有限公司 | Preparation method for reinforced low-resilience and low-alkaline liquid concrete accelerator |
| CN107572856A (en) * | 2017-10-09 | 2018-01-12 | 常州琨瑶纺织品有限公司 | A kind of green alkali-free liquid concrete accelerator and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748533A (en) * | 2019-03-04 | 2019-05-14 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | A kind of core master batch and preparation method thereof for alkali-free liquid setting accelerator |
| CN110330255A (en) * | 2019-07-02 | 2019-10-15 | 安徽海螺新材料科技有限公司 | It is a kind of to promote solidifying type liquid grinding aid and preparation method thereof |
| CN110330255B (en) * | 2019-07-02 | 2021-08-31 | 安徽海螺新材料科技有限公司 | Coagulation-promoting liquid grinding aid and preparation method thereof |
| CN113087441A (en) * | 2021-03-05 | 2021-07-09 | 山西佳维新材料股份有限公司 | Fluoride-free liquid alkali-free accelerator and preparation method and application thereof |
| CN113480226A (en) * | 2021-08-02 | 2021-10-08 | 江西立晶新材料科技有限公司 | Liquid alkali-free accelerator and preparation method and application thereof |
| CN116283024A (en) * | 2023-03-21 | 2023-06-23 | 安宁市云洲新型建材有限公司 | Environment-friendly liquid alkali-free accelerator and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109293269B (en) | 2021-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109293269A (en) | A kind of preparation method of early-strength alkali-free liquid accelerator | |
| CN107200497A (en) | A kind of chlorine-free alkali-free liquid accelerating agent and preparation method thereof | |
| CN105174796B (en) | A kind of alkali-free liquid concrete accelerator and preparation method thereof | |
| CN104446090B (en) | A kind of alkali-free liquid accelerator of durability and preparation method thereof | |
| CN109399999B (en) | Green high-early-strength low-alkali liquid accelerator and preparation method thereof | |
| CN102924019B (en) | High-strength micro-expansive grouting material and its preparation method | |
| CN110734242B (en) | Sprayed concrete alkali-free liquid accelerator for alpine regions and preparation method thereof | |
| CN109231871A (en) | A kind of low-mix quantity high performance alkali-free chlorine-free liquid accelerator and preparation method thereof | |
| CN104119021B (en) | High efficiency water reducing agent | |
| CN107840593A (en) | A kind of gunite concrete early-strength alkali-free liquid setting accelerator and preparation method thereof | |
| CN107459278A (en) | A kind of gunite concrete low-alkali liquid quick-setting agent and preparation method thereof | |
| CN111646728A (en) | Quick-setting high-strength alkali-free liquid accelerator | |
| CN110104987A (en) | A kind of high early-strength alkali-free liquid accelerator and its preparation method and application | |
| CN104030595A (en) | Compound concrete admixture with early strength and water reduction functions, and preparation method and application thereof | |
| CN108358591B (en) | Building material composition containing aeolian sand and preparation method thereof | |
| CN110330255B (en) | Coagulation-promoting liquid grinding aid and preparation method thereof | |
| CN112521113B (en) | Low-temperature hydration hardening gel material and preparation method and application thereof | |
| CN108191293B (en) | Low-temperature curing agent for concrete | |
| CN110615638A (en) | Low-temperature-resistant liquid alkali-free setting accelerator and preparation method thereof | |
| CN115403294B (en) | High-stability alkali-free chlorine-free fluorine-free liquid accelerator and preparation method thereof | |
| CN115466075A (en) | Preparation method and application of alkali-free and fluorine-free liquid accelerator | |
| CN110436811A (en) | A kind of chlorine-free alkali-free liquid accelerating agent and preparation method thereof | |
| CN113582573A (en) | Accelerating agent and preparation method and application thereof | |
| CN110746549B (en) | Ultra-long slow-release polycarboxylic slump retaining agent and preparation method thereof | |
| CN114573267A (en) | Alkali-free, chlorine-free and fluorine-free environment-friendly liquid accelerator, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 276000 north of the intersection of Wenquan road and Fenghuang street, Fenghuangling sub district office, Hedong, Linyi City, Shandong Province Patentee after: Linyi conch New Material Technology Co.,Ltd. Address before: 276000 east section of Renmin Road, Hedong District, Linyi City, Shandong Province Patentee before: LINYI HONGYI TECHNOLOGY DEVELOPMENT Co.,Ltd. |
|
| CP03 | Change of name, title or address |