CN109265043B - Alkali-free liquid accelerator adopting electrolytic method and preparation method thereof - Google Patents
Alkali-free liquid accelerator adopting electrolytic method and preparation method thereof Download PDFInfo
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- CN109265043B CN109265043B CN201811417726.XA CN201811417726A CN109265043B CN 109265043 B CN109265043 B CN 109265043B CN 201811417726 A CN201811417726 A CN 201811417726A CN 109265043 B CN109265043 B CN 109265043B
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- alkali
- free liquid
- liquid accelerator
- aluminum
- accelerator
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
-
- 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
Abstract
The invention provides an alkali-free liquid accelerator adopting an electrolytic method, which comprises the following components in percentage by mass: aluminum alloy: 2-3%, aluminum sulfate: 40-45%, magnesium fluosilicate: 6-8%, hydrofluoric acid: 2-4%, reinforcing components: 7-10%, alcohol amine: 0.1-0.5%, and the balance of water, which accounts for 100%; the invention also provides a preparation method of the alkali-free liquid accelerator, which comprises the following steps: (1) preparing an electrolyte; (2) preparing aluminum hydroxide gel; (3) preparing polyaluminium sulfate; (4) preparing an alkali-free liquid accelerator; the invention adopts electrolytic method to prepare polymeric aluminum sulfate type liquid alkali-free accelerator, without alkalizer, and takes aluminum alloy as anode, electrifys to oxidize the aluminum alloy to generate aluminum hydroxide gel, and reacts with aluminum sulfate in the solution to generate polymeric aluminum sulfate solution. Compared with other similar products in the market, the product has good adaptability to different types of cement and good product stability, is an alkali-free liquid accelerator with superior performance, and can be widely applied to projects such as tunnels, bridges, rush repairs and the like.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an alkali-free liquid accelerator adopting an electrolytic method and a preparation method thereof.
Background
The setting accelerator is a setting regulator capable of accelerating the setting and hardening speed of concrete, and can make concrete set and hardened in a short time. The accelerator has wide application in sprayed concrete, sprayed mortar, rush repair reinforcement engineering and grouting water-stop concrete, and becomes an essential additive. In recent years, the wet concrete spraying process has been widely used because of its advantages of good construction environment, low resilience, high construction efficiency, etc., and the accelerator used in conjunction with the construction process is usually a liquid accelerator.
The liquid accelerator for wet shotcrete includes an alkali accelerator and an alkali-free accelerator. The alkali-aggregate-free concrete accelerator is high in alkali content, easily causes physical damage to constructors, easily induces alkali-aggregate reaction, and adversely affects later strength and durability of concrete. Therefore, the alkali-free liquid accelerator is the mainstream accelerator development direction in the world in consideration of the influence of the accelerator on mechanical properties, construction performance, construction method and the like of the sprayed concrete.
The mainstream liquid accelerator in the market at present is mainly polymeric aluminum sulfate, the main component of the liquid accelerator is polymeric aluminum sulfate solution, and the polymeric aluminum sulfate has high solubility and good stability. Polyaluminium sulfate can react with cement to generate a large amount of fine needle-like ettringite and intermediate product secondary gypsum, thereby causing the cement to be quickly solidified. The polyaluminium sulfate is mainly used in the field of water purification at present and is used as a flocculating agent, and the synthesis mechanism is essentially to introduce active Al (OH) into an aluminium sulfate solution3Gel, active Al (OH)3Gel energy and Al in aluminum sulfate solution3+Reacting to generate various polymeric hydroxyl complex ions, wherein the reaction formula is as follows:
xAl3++yAl(OH)3(colloid) ═ Al(x+y)(OH)3y 3x+
In the field of accelerating agents, the preparation methods of the existing polyaluminium sulfate mainly comprise two methods:
firstly, pre-preparing active Al (OH)3Adding the gel into an aluminum sulfate solution to prepare a polyaluminum sulfate solution, wherein the polyaluminum sulfate solution is currently commercially available as active Al (OH)3Gel products are few and generally need to be prefabricated. Patent publication No. CN105271867A discloses a novel alkali-free liquid accelerator based on synthetic polyaluminium sulfate, which is prepared by reacting ammonia water with an aluminium sulfate solution to obtain an active aluminium hydroxide gel, filtering, drying, grinding, and addingAdding into aluminum sulfate solution to obtain polyaluminum sulfate, preformed active Al (OH)3The gel method has complex process and complicated steps, and a large amount of byproducts and waste water are discharged;
secondly, a small amount of alkalizer is introduced into the aluminum sulfate solution, so that part of aluminum sulfate in the solution reacts with the alkalizer to generate active Al (OH)3Gel, the newly generated active aluminum hydroxide gel reacts with the rest aluminum sulfate directly in the solution to generate polyaluminium sulfate solution, and Al in the polyaluminium sulfate solution3+Is the main coagulation accelerating component, and the excessive concentration of sulfate radical can affect the solution stability of the polyaluminium sulfate. Patent document with publication number CN102219426A discloses a low alkali liquid accelerator and a preparation method thereof, wherein the low alkali liquid accelerator comprises the following components in percentage by mass: 40-60% of aluminum sulfate, 6-12% of sodium aluminate, 0-0.2% of stabilizer and the balance of water. Al in the method3+Mainly from aluminium sulphate, often resulting in an excessive sulphate content in the accelerator, Al3+The content is relatively low, so that the solid content of the accelerator is limited, and the doping amount of the prepared polyaluminium sulfate accelerator is too large.
In view of the above, the present inventors have specially designed an alkali-free liquid accelerator using electrolysis and a method for preparing the same, and have thus developed the present application.
Disclosure of Invention
Aiming at the defects of the preparation method of the polyaluminium sulfate in the field of the accelerating agent, which are mentioned in the background art, the technical scheme of the invention is as follows:
the invention provides an alkali-free liquid accelerator adopting an electrolytic method, which comprises the following components in percentage by mass:
aluminum alloy: 2-3%;
aluminum sulfate: 40-45%;
magnesium fluosilicate: 6-8%;
hydrofluoric acid: 2-4%;
the reinforcing component: 7-10%;
alcohol amine: 0.1-0.5%;
the balance of water, which is 100 percent in total.
Further, the aluminum alloy is used as an anode of an electrolytic method, wherein the Al content is 95-98%.
Further, the aluminum sulfate is industrial grade aluminum sulfate octadecahydrate, wherein Al2O3The content is more than 15 percent.
Further, the magnesium fluosilicate is industrial grade magnesium fluosilicate hexahydrate.
Further, the hydrofluoric acid is an industrial grade hydrofluoric acid solution, and the concentration of the hydrofluoric acid solution is 40%.
Further, the reinforcing component can be any one of formic acid, acetic acid or oxalic acid, and formic acid is preferred.
Further, the alcohol amine may be triethanolamine or diethanolamine, preferably triethanolamine.
The invention also provides a preparation method of the alkali-free liquid accelerator by adopting an electrolytic method, which comprises the following steps:
(1) preparing an electrolyte: heating water to 70-80 ℃, dissolving aluminum sulfate in the water, keeping the temperature and stirring to form the required electrolyte;
(2) preparing aluminum hydroxide gel: taking aluminum alloy as an anode and an inert electrode as a cathode, inserting the two electrodes into electrolyte, electrifying, oxidizing the metered aluminum alloy anode by controlling current and electrifying time, dissolving the aluminum alloy anode in the electrolyte, and generating aluminum hydroxide gel;
(3) preparation of polyaluminium sulfate: powering off, taking out the electrode, keeping the temperature of 70-80 ℃ and stirring for 30min to enable aluminum sulfate in the solution to react with aluminum hydroxide gel to generate polyaluminum sulfate;
(4) preparing an alkali-free liquid accelerator: respectively and sequentially adding magnesium fluosilicate, hydrofluoric acid, a reinforcing component and alcohol amine, and respectively stirring.
Further, in the step 2, hydrogen generated by the cathode is exhausted through an air exhaust device.
Further, the step 4 sequentially comprises the following specific steps:
a. adding magnesium fluosilicate, and stirring for 30 min;
b. adding hydrofluoric acid, stirring for 30min, adjusting the pH value of the accelerator to 2-3 by the hydrofluoric acid, improving the stability of the accelerator, improving the content of fluoride ions and enhancing the accelerating effect;
c. adding the reinforcing component and alcohol amine, and stirring for 10-20 min to obtain the alkali-free liquid accelerator.
The invention relates to a method for preparing an alkali-free liquid accelerator by adopting an electrolytic method, which adopts the electrolytic method, takes an aluminum alloy as an anode, and is electrified to accelerate the oxidation and dissolution of the anode to generate aluminum hydroxide gel, the reaction of general aluminum metal and water is easy to passivate, compact aluminum oxide is generated on the surface to hinder the further reaction; and the active Al (OH) is introduced by adopting an electrolytic method3The gel can flexibly adjust Al in the polyaluminium sulfate solution3+And SO4 2-The proportion of (A) is not needed to be additionally added with an alkalizer, and the influence of the introduction of excessive sulfate radicals on the stability of the solution is avoided. In the invention, aluminum hydroxide gel is introduced by taking the aluminum alloy sacrificial anode as a material to prepare the high Al alloy3+The polyaluminum sulfate type alkali-free liquid accelerator with the content has simple preparation method; the prepared alkali-free liquid accelerator has good stability and can be stably stored for 6 months; the mixing amount of the accelerator is low, and the setting time and the mortar strength can meet the requirements of JC477-2005 accelerator for sprayed concrete on first-class products under the condition that the mixing amount is 5-8 percent (mass of cement).
Detailed Description
The technical solution of the present invention is further illustrated by the following examples. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The invention firstly provides an alkali-free liquid accelerator adopting an electrolytic method, which comprises the following components in percentage by mass:
aluminum alloy: 2-3%, aluminum sulfate: 40-45%, magnesium fluosilicate: 6-8%, hydrofluoric acid: 2-4%, reinforcing components: 7-10%, alcohol amine: 0.1-0.5%, and the balance of water, which accounts for 100%.
The aluminum alloy is used as an anode of an electrolytic method, aluminum hydroxide is introduced into a sacrificial anode, and the content of Al is 95-98%; the aluminum sulfate is industrial grade aluminum sulfate octadecahydrate, wherein Al2O3The content is more than 15 percent; the magnesium fluosilicate is industrial grade magnesium fluosilicate hexahydrate; the hydrofluoric acid is an industrial grade hydrofluoric acid solution, and the concentration of the hydrofluoric acid is 40%; the reinforcing component can be any one of formic acid, acetic acid or oxalic acid, and formic acid is preferred; the alcohol amine can be triethanolamine or diethanolamine, preferably triethanolamine.
The invention also provides a preparation method of the alkali-free liquid accelerator by adopting an electrolytic method, which comprises the following steps:
(1) preparing an electrolyte: heating water to 70-80 ℃, dissolving aluminum sulfate in the water, keeping the temperature and stirring to form the required electrolyte;
(2) preparing aluminum hydroxide gel: taking aluminum alloy as an anode and an inert electrode as a cathode, inserting the two electrodes into electrolyte, electrifying, oxidizing the metered aluminum alloy anode by controlling current and electrifying time, dissolving the aluminum alloy anode into the electrolyte to generate aluminum hydroxide gel, and simultaneously discharging hydrogen generated by the cathode through an air draft device;
(3) preparation of polyaluminium sulfate: powering off, taking out the electrode, keeping the temperature of 70-80 ℃ and stirring for 30min to enable aluminum sulfate in the solution to react with aluminum hydroxide gel to generate polyaluminum sulfate;
(4) preparing an alkali-free liquid accelerator: respectively and sequentially adding magnesium fluosilicate, hydrofluoric acid, a reinforcing component and alcohol amine, and respectively stirring.
Wherein, the step 4 comprises the following concrete steps in sequence:
a. adding magnesium fluosilicate, and stirring for 30 min;
b. adding hydrofluoric acid, stirring for 30min, adjusting the pH value of the accelerator to 2-3 by the hydrofluoric acid, improving the stability of the accelerator, improving the content of fluoride ions and enhancing the accelerating effect;
c. adding the reinforcing component and alcohol amine, and stirring for 10-20 min to obtain the alkali-free liquid accelerator.
Example 1
An alkali-free liquid accelerator adopting an electrolytic method comprises the following components in percentage by mass: 2.8% of aluminum alloy, 40% of aluminum sulfate, 7% of magnesium fluosilicate, 3% of hydrofluoric acid, 8% of formic acid, 0.2% of triethanolamine and the balance of water.
The preparation method comprises the following steps:
(1) preparing an electrolyte: heating water to 70-80 ℃, dissolving aluminum sulfate in the water, keeping the temperature and stirring to form the required electrolyte;
(2) preparing aluminum hydroxide gel: taking aluminum alloy as an anode and an inert electrode as a cathode, inserting the two electrodes into electrolyte, electrifying, oxidizing the metered aluminum alloy anode by controlling current and electrifying time, dissolving the aluminum alloy anode into the electrolyte to generate aluminum hydroxide gel, and simultaneously discharging hydrogen generated by the cathode through an air draft device;
(3) preparation of polyaluminium sulfate: powering off, taking out the electrode, keeping the temperature of 70-80 ℃ and stirring for 30min to enable aluminum sulfate in the solution to react with aluminum hydroxide gel to generate polyaluminum sulfate;
(4) preparing an alkali-free liquid accelerator: firstly, adding magnesium fluosilicate, and stirring for 30 min; then adding hydrofluoric acid, stirring for 30min, adjusting the pH value of the accelerator to 2-3 by the hydrofluoric acid, improving the stability of the accelerator, improving the content of fluoride ions and enhancing the accelerating effect; and finally, adding the reinforcing component and alcohol amine, and stirring for 10-20 min to obtain the alkali-free liquid accelerator.
Example 2
An alkali-free liquid accelerator prepared by an electrolytic method comprises the following components in percentage by mass: 3% of aluminum alloy, 43% of aluminum sulfate, 7% of magnesium fluosilicate, 3% of hydrofluoric acid, 9% of formic acid, 0.3% of diethanol amine and the balance of water.
The preparation is as described in example 1.
Example 3
An alkali-free liquid accelerator prepared by an electrolytic method comprises the following components in percentage by mass: 3% of aluminum alloy, 45% of aluminum sulfate, 8% of magnesium fluosilicate, 3.5% of hydrofluoric acid, 8% of oxalic acid, 0.5% of diethanolamine and the balance of water.
The preparation is as described in example 1.
The setting time of the cement paste and the compressive strength of cement mortar are tested according to the requirements of JC477-2005 accelerator for sprayed concrete, and the test results are shown in Table 1:
TABLE 1 test results of the examples
As can be seen from Table 1, the alkali-free liquid accelerator provided by the invention can enable the setting time of a cement paste to meet the requirements that the initial setting time is less than 5 minutes and the final setting time is less than 12 minutes under the condition of 5-8% of doping amount, the 1d strength of the mortar is greater than 7MPa, the 28d compressive strength ratio is greater than 95%, and the alkali-free liquid accelerator has very good cement adaptability and can enable different types of cement to meet the construction requirements of sprayed concrete. Therefore, the polyaluminum sulfate type liquid alkali-free accelerator is prepared by an electrolytic method, an alkalizer is not needed, aluminum alloy is used as an anode, the aluminum alloy is electrified to be oxidized to generate aluminum hydroxide gel, and the aluminum hydroxide gel reacts with aluminum sulfate in the solution to generate polyaluminum sulfate solution.
In summary, the method for preparing the alkali-free liquid accelerator by adopting the electrolytic method adopts the electrolytic method, takes the aluminum alloy as the anode, and energizes to accelerate the oxidation and dissolution of the anode to generate aluminum hydroxide gel, the reaction of general aluminum metal and water is easy to passivate, compact aluminum oxide is generated on the surface, and the further proceeding of the reaction is hindered; and the active Al (OH) is introduced by adopting an electrolytic method3Gel, KelinLive-regulated polyaluminium sulfate solution of Al3+And SO4 2-The proportion of (A) is not needed to be additionally added with an alkalizer, and the influence of the introduction of excessive sulfate radicals on the stability of the solution is avoided. In the invention, aluminum hydroxide gel is introduced by taking the aluminum alloy sacrificial anode as a material to prepare the high Al alloy3+The polyaluminum sulfate type alkali-free liquid accelerator with the content has simple preparation method; the prepared alkali-free liquid accelerator has good stability and can be stably stored for 6 months; the mixing amount of the accelerator is low, and the setting time and the mortar strength can meet the requirements of JC477-2005 accelerator for sprayed concrete on first-class products under the condition that the mixing amount is 5-8 percent (mass of cement).
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (9)
1. An alkali-free liquid accelerator adopting an electrolytic method is characterized by comprising the following components in percentage by mass:
aluminum alloy: 2-3%;
aluminum sulfate: 40-45%;
magnesium fluosilicate: 6-8%;
hydrofluoric acid: 2-4%;
the reinforcing component: 7-10%;
alcohol amine: 0.1-0.5%;
the balance of water, which is 100 percent in total;
the preparation method of the alkali-free liquid accelerator comprises the following steps:
(1) preparing an electrolyte: heating water to 70-80 ℃, dissolving aluminum sulfate in the water, keeping the temperature and stirring to form the required electrolyte;
(2) preparing aluminum hydroxide gel: taking aluminum alloy as an anode and an inert electrode as a cathode, inserting the two electrodes into electrolyte, electrifying, oxidizing the metered aluminum alloy anode by controlling current and electrifying time, dissolving the aluminum alloy anode in the electrolyte, and generating aluminum hydroxide gel;
(3) preparation of polyaluminium sulfate: powering off, taking out the electrode, keeping the temperature of 70-80 ℃ and stirring for 30min to enable aluminum sulfate in the solution to react with aluminum hydroxide gel to generate polyaluminum sulfate;
(4) preparing an alkali-free liquid accelerator: respectively and sequentially adding magnesium fluosilicate, hydrofluoric acid, a reinforcing component and alcohol amine, and respectively stirring.
2. The alkali-free liquid accelerator according to claim 1, wherein the aluminum alloy is used as an anode of an electrolytic process, and the content of Al is 95-98%.
3. The alkali-free liquid accelerator for electrolysis according to claim 1, wherein the aluminum sulfate is industrial grade aluminum sulfate octadecahydrate, wherein Al is aluminum sulfate octadecahydrate2O3The content is more than 15 percent.
4. The alkali-free liquid accelerator by electrolysis according to claim 1, wherein the magnesium fluosilicate is industrial grade magnesium fluosilicate hexahydrate.
5. The alkali-free liquid accelerator according to claim 1, wherein the hydrofluoric acid is a technical hydrofluoric acid solution with a concentration of 40%.
6. The alkali-free liquid accelerator according to claim 1, wherein the reinforcing component is any one of formic acid, acetic acid and oxalic acid.
7. The alkali-free liquid accelerator according to claim 1, wherein the alcohol amine is triethanolamine or diethanolamine.
8. The alkali-free liquid accelerator for electrolysis according to claim 1, wherein hydrogen generated at the cathode in step 2 is exhausted by an air exhaust device.
9. The alkali-free liquid accelerator adopting the electrolytic method according to claim 1, wherein the step 4 comprises the following specific steps in sequence:
a. adding magnesium fluosilicate, and stirring for 30 min;
b. adding hydrofluoric acid, stirring for 30min, adjusting the pH value of the accelerator to 2-3 by the hydrofluoric acid, improving the stability of the accelerator, improving the content of fluoride ions and enhancing the accelerating effect;
c. adding the reinforcing component and alcohol amine, and stirring for 10-20 min to obtain the alkali-free liquid accelerator.
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| CN87103213A (en) * | 1987-04-30 | 1987-12-30 | 西北电讯工程学院 | Form the method for oxide film in the aluminium electrolyticing coloring technology |
| CN102312265A (en) * | 2011-09-22 | 2012-01-11 | 珠海市赛日包装材料有限公司 | Preparation method for anode oxidation film of aluminum or aluminum alloy |
| CN106082763A (en) * | 2016-06-14 | 2016-11-09 | 山东远利华矿用装备有限公司 | A kind of alkali-free liquid accelerating agent and its preparation method and application method |
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| CN87103213A (en) * | 1987-04-30 | 1987-12-30 | 西北电讯工程学院 | Form the method for oxide film in the aluminium electrolyticing coloring technology |
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| CN106082763A (en) * | 2016-06-14 | 2016-11-09 | 山东远利华矿用装备有限公司 | A kind of alkali-free liquid accelerating agent and its preparation method and application method |
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