CN113200702B - Alkali-free liquid accelerator containing biological enzyme and preparation method thereof - Google Patents
Alkali-free liquid accelerator containing biological enzyme and preparation method thereof Download PDFInfo
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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
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- C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
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- 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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Abstract
The invention belongs to the field of novel building materials, and discloses an alkali-free liquid accelerator containing biological enzyme, which is an emulsion preparation and comprises the following components in percentage by mass: fluosilicic acid: 16% -20%, aluminum hydroxide: 3% -6%, phosphoric acid: 0.1-0.2%, aluminum sulfate: 38% -42%, zinc oxide: 0.02% -0.07%, magnesium hydroxide: 5% -10%, sodium fluoride: 0.1% -0.4%, betaine: 0.1-0.4%, crystal inhibitor: 1-4%, polycarboxylic acid high-performance water reducing agent: 0.04-0.07%, home-made biological enzyme: 0.2% -0.5%, tap water: 18 to 37 percent. The invention uses the coordinated fluosilicic acid to replace fluosilicic acid, solves the problem of overproof fluorine ions, and can sterilize and disinfect and protect the health of operators by adding the homemade biological enzyme. The prepared accelerator is simple to produce, non-toxic and pollution-free, and has high 1d compressive strength and good product placement stability, so that the accelerator has the advantages of no collapse of later compressive strength, good durability, low resilience and the like.
Description
Technical Field
The invention belongs to the field of novel building materials, and particularly relates to an alkali-free liquid accelerator containing biological enzyme and a preparation method thereof.
Background
The accelerator is one of indispensable admixtures for sprayed concrete, and is widely applied to the fields of underground engineering, mine engineering and various support engineering. With the vigorous development of the high-speed rail industry in China, higher requirements are put forward on the construction process, the supporting quality and the working environment of the shotcrete for the primary support of the tunnel, the wet spraying process is required to be adopted for the shotcrete for the primary support in the railway industry, and the accelerator is not harmful to operators. Therefore, the traditional powder accelerator is developed into a high-alkali liquid accelerator and a low-alkali liquid accelerator which are prepared by reacting aluminum hydroxide and sodium hydroxide, but the liquid accelerators contain strong alkaline substances, have strong corrosiveness, are easy to hurt constructors, easily cause the strength reduction of concrete, surface cracking, peeling and even collapse to cause safety accidents, and seriously lose the strength of the concrete at the high later period of resilience, and seriously affect the durability of sprayed concrete. The alkali-free liquid accelerator just compensates for part of the defects, so that various hydrofluoric acid, fluosilicic acid and organic acid are used for neutralizing aluminum hydroxide, aluminum sulfate, magnesium fluosilicate, sodium fluoride, a neutralizing agent (for adjusting the pH value of the alkali-free liquid accelerator) and the like are added, and then the alkali-free liquid accelerator supplemented with organic alcohol amine and a suspending agent stabilizer is used for producing the alkali-free liquid accelerator. Therefore, the development of an environment-friendly alkali-free liquid accelerator meeting high standard requirements is urgent.
Disclosure of Invention
The invention provides an alkali-free liquid accelerator containing biological enzyme and a preparation method thereof, aiming at the problems that the existing alkali-free liquid accelerator is strong in corrosivity, poor in adaptability, and the 1d compressive strength cannot meet the standard requirement. The method of the invention prepares the alkali-free liquid accelerator containing the biological enzyme by introducing the self-made biological enzyme, which not only can improve the strength, the product stability and the field performance capability of the alkali-free liquid accelerator, but also can sterilize and disinfect and protect the health of operators.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an alkali-free liquid accelerator containing biological enzyme, which comprises the following components in percentage by mass: fluosilicic acid: 16% -20%, aluminum hydroxide: 3% -6%, phosphoric acid: 0.1-0.2%, aluminum sulfate: 38% -42%, zinc oxide: 0.02% -0.07%, magnesium hydroxide: 5% -10%, sodium fluoride: 0.1% -0.4%, betaine: 0.1-0.4%, crystal inhibitor: 1-4%, polycarboxylic acid high-performance water reducing agent: 0.04-0.07%, home-made biological enzyme: 0.2% -0.5%, tap water: 18 to 37 percent.
Further, the homemade biological enzyme is prepared by the following method, wherein the homemade biological enzyme comprises the following components in percentage by mass: 30% of crushed and cleaned fruit and vegetable plants, 1% of liquorice, 0.5% of vitamin, 5% of brown sugar and 63.5% of tap water are placed in a clean container, the container is sealed and placed for 4-6 months at 15-30 ℃, air is periodically discharged during the period, and the obtained clear liquid after filtration is the home-made biological enzyme. The self-made biological enzyme can be used for cement-based gelling materials and has the functions of enhancing and improving performance.
Further, the fluosilicic acid is obtained by coordinating with the nano silicon dioxide, and the specific coordination process is that the nano silicon dioxide is added into the fluosilicic acid, stirred for 30min, and kept stand for 24h, and then supernatant is obtained. The mass ratio of the nano silicon dioxide to the fluosilicic acid is 5-10: 100. the content of hydrofluoric acid can be reduced by carrying out coordination on the fluosilicic acid, the nanometer silicon dioxide and the silicic acid can be selected for coordination, and the nanometer silicon dioxide is preferably selected for the invention.
The phosphoric acid is industrial grade, can promote the reaction of the fluosilicic acid and the aluminum hydroxide, is beneficial to the stability of the system, can also select citric acid, acetic acid, formic acid and lactic acid, and is preferred in the invention.
The aluminum sulfate is industrial grade, white crystal or slightly yellowish, contains 16 molecular crystal water and is easy to dissolve in water.
The zinc oxide, the magnesium hydroxide and the sodium fluoride are all in industrial grade, have the functions of regulating the pH value and improving the 1d compressive strength of the alkali-free liquid accelerator in a system, and have a stabilizing effect on the system. And also can be magnesium silicate, potassium dihydrogen phosphate, potassium hydroxide, magnesium oxide, sodium metaaluminate, magnesium fluosilicate and zinc fluosilicate, and the invention preferably selects zinc oxide, magnesium hydroxide and sodium fluoride.
The betaine (C) 5 H 11 NO 2 ) The invention adopts feed-grade betaine as a surfactant, mainly plays roles in regulating the pH value and stabilizing a system, ensures the stability of the product in placement, has a certain enhancing effect, and can also select other suspending agent stabilizers.
The crystal inhibitor is acetone, ethanol, methanol and the like, which are all industrial grade, wherein the acetone has the best effect but belongs to dangerous goods, and therefore, the methanol is preferred in the invention.
The polycarboxylic acid high-performance water reducing agent is a standard type sold in the market, the solid content is 40%, and the water reducing rate is 26%. The polycarboxylic acid high-performance water reducing agent has a low addition proportion, and is mainly used for colloid particles in a dispersion system so as to avoid agglomeration, delamination and precipitation to cause poor product stability.
The invention also provides a preparation method of the alkali-free liquid accelerator containing the biological enzyme, which comprises the following steps:
step 1, adding nano silicon dioxide into fluosilicic acid, stirring for 30min, standing for 24h, and taking clear liquid to obtain coordinated fluosilicic acid;
step 2, adding tap water and aluminum hydroxide into a container, stirring the mixture into paste at 50-70 ℃, then sequentially adding phosphoric acid and coordinated fluosilicic acid at the speed of 400-600r/min while stirring, and reacting for 30-40 min;
step 3, adding tap water, aluminum sulfate, zinc oxide, magnesium hydroxide and sodium fluoride at the temperature of 60-80 ℃ and the speed of 300-; the materials are mixed and added, and are not easy to agglomerate, and can also be added by other modes, and the materials are not easy to agglomerate;
step 4, when the temperature is reduced to 45-50 ℃, adding betaine, and continuing stirring until the betaine is completely dissolved;
step 5, when the temperature is reduced to 35-45 ℃, adding a crystal inhibitor and a polycarboxylic acid high-performance water reducing agent, and stirring for 15-20min at the stirring speed of 550-650 r/min;
and 6, when the temperature is reduced to 30-40 ℃, adding the self-made biological enzyme, and continuously stirring for 10-20min to obtain a white emulsion finished product, namely the alkali-free liquid accelerator containing the biological enzyme.
Further, the mass ratio of the nano silicon dioxide to the fluosilicic acid in the step 1 is 5-10: 100, respectively; in the step 2, the mass ratio of tap water to aluminum hydroxide is 1: 2; in the method, the mass ratio of total tap water, aluminum hydroxide, phosphoric acid, coordinated fluosilicic acid, aluminum sulfate, zinc oxide, magnesium hydroxide, sodium fluoride, betaine, a crystal inhibitor, a polycarboxylic acid high-performance water reducing agent and self-made biological enzyme used in steps 2 and 3 is 18-37: 3-6: 0.1-0.2: 16-20: 38-42: 0.02-0.07: 5-10: 0.1-0.4: 0.1-0.4: 1-4: 0.04-0.07: 0.2 to 0.5.
Further, the step 2 and the step 3 may be performed separately, and then the solution obtained in the step 2 is added to the solution obtained in the step 3 while stirring, and other steps are not changed.
Compared with the prior art, the invention has the following advantages:
1. the invention discloses an alkali-free liquid accelerator containing biological enzyme, which is an emulsion preparation, is simple to produce, nontoxic and pollution-free, has high compressive strength at 1d and good product placement stability, so that the accelerator has the advantages of no collapse of the compressive strength at the later stage, good durability, low resilience and the like.
2. The method ensures the placement stability of the alkali-free liquid accelerator product through the multi-component superposition effect, and improves the 1d compressive strength, thereby improving the expressive force of site construction, reducing the rebound rate, and ensuring that the later strength is not shrunk. In addition, the coordination fluosilicic acid is used for replacing fluosilicic acid, so that the problem that the fluorine ions exceed the standard is solved, and the adjustability and controllability of the condensation time are ensured.
Detailed Description
The following examples are illustrative of the preferred embodiments of the present invention, but the present invention is not limited to the following examples, and it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and the present invention is included in the protection scope of the present invention.
The fluosilicic acid in the following examples is the fluosilicic acid coordinated by nano-silica.
Example 1
The alkali-free liquid accelerator containing the biological enzyme is prepared from the following raw materials in percentage by mass: fluosilicic acid: 16 percent; aluminum hydroxide: 3 percent; phosphoric acid: 0.1 percent; aluminum sulfate: 38 percent; zinc oxide: 0.03 percent; magnesium hydroxide: 5 percent; sodium fluoride: 0.1 percent; betaine: 0.1 percent; crystal inhibitor: 1 percent; polycarboxylic acid high-performance water reducing agent: 0.04 percent; self-made biological enzyme: 0.2 percent; tap water: 36.43 percent;
example 2
The alkali-free liquid accelerator containing the biological enzyme is prepared from the following raw materials in percentage by mass: fluosilicic acid: 18 percent; aluminum hydroxide: 5 percent; phosphoric acid: 0.15 percent; aluminum sulfate: 40 percent; zinc oxide: 0.05 percent; magnesium hydroxide: 7 percent; sodium fluoride: 0.2 percent; betaine: 0.2 percent; crystal inhibitor: 2 percent; polycarboxylic acid high-performance water reducing agent: 0.05 percent; self-made biological enzyme: 0.3 percent; tap water: 27.05 percent;
example 3
The alkali-free liquid accelerator containing the biological enzyme is prepared from the following raw materials in percentage by mass: fluosilicic acid: 19 percent; aluminum hydroxide: 4 percent; phosphoric acid: 0.17 percent; aluminum sulfate: 41 percent; zinc oxide: 0.06 percent; magnesium hydroxide: 8 percent; sodium fluoride: 0.3 percent; betaine: 0.3 percent; crystal inhibitor: 3 percent; polycarboxylic acid high-performance water reducing agent: 0.06 percent; self-made biological enzyme: 0.4 percent; tap water: 23.71 percent;
example 4
The alkali-free liquid accelerator containing the biological enzyme is prepared from the following raw materials in percentage by mass: fluosilicic acid: 20 percent; aluminum hydroxide: 6 percent; phosphoric acid: 0.2 percent; aluminum sulfate: 40 percent; zinc oxide: 0.07 percent; magnesium hydroxide: 10 percent; sodium fluoride: 0.4 percent; betaine: 0.4 percent; crystal inhibitor: 4 percent; polycarboxylic acid high-performance water reducing agent: 0.07 percent; self-made biological enzyme: 0.5 percent; tap water: 18.36 percent;
example 5: (verification of the action of the biological enzyme without adding the biological enzyme on the basis of example 2)
The alkali-free liquid accelerator containing the biological enzyme is prepared from the following raw materials in percentage by mass: fluosilicic acid: 18 percent; aluminum hydroxide: 5 percent; phosphoric acid: 0.15 percent; aluminum sulfate: 40 percent; zinc oxide: 0.05 percent; magnesium hydroxide: 7 percent; sodium fluoride: 0.2 percent; betaine: 0.2 percent; crystal inhibitor: 2 percent; polycarboxylic acid high-performance water reducing agent: 0.05 percent; self-made biological enzyme: 0 percent; tap water: 27.35 percent;
example 6
The preparation method of the alkali-free liquid accelerator containing the biological enzyme comprises the following steps:
step 1, adding tap water and aluminum hydroxide which account for half of the mass of the aluminum hydroxide into a container, starting a heating device, stirring into paste, gradually adding coordinated fluosilicic acid while stirring, controlling the speed of adding the fluosilicic acid to avoid boiling overflow, simultaneously adding phosphoric acid, controlling the heating temperature at 60 ℃, stopping heating, and reacting for 35min, wherein the exothermic temperature of the neutralization reaction can reach 90-100 ℃, and the stirring speed is controlled at 500 r/min.
Step 2, adding the rest tap water, continuously stirring and heating, gradually adding aluminum sulfate, zinc oxide, magnesium hydroxide and sodium fluoride, controlling the temperature at 70 ℃ and the stirring speed at 400 r/min; when the solution reached a milky white liquid (the solid was completely dissolved), the heating was stopped and the stirring was continued.
Step 3, when the temperature is reduced to 48 ℃, adding the betaine, and continuing stirring until the betaine is completely dissolved;
step 4, when the temperature is reduced to 40 ℃, adding a crystal inhibitor and a polycarboxylic acid high-performance water reducing agent, and stirring for 18min at a stirring speed of 600 r/min;
and 5, when the temperature is reduced to 35 ℃, adding the self-made biological enzyme, and continuously stirring for 15min to obtain a white emulsion finished product, namely the alkali-free liquid accelerator containing the biological enzyme.
Example 7
The preparation method of the alkali-free liquid accelerator containing the biological enzyme comprises the following steps:
step 1, adding tap water and aluminum hydroxide which account for half of the mass of the aluminum hydroxide into a container, starting a heating device, stirring the mixture into paste, gradually adding coordinated fluosilicic acid while stirring, controlling the speed of adding the fluosilicic acid to avoid boiling overflow, simultaneously adding phosphoric acid, controlling the heating temperature to be 50 ℃, stopping heating, and controlling the stirring speed to be 400r/min and reacting for 30min because the heat release temperature of the neutralization reaction can reach 90-100 ℃.
Step 2, adding the rest tap water, continuously stirring and heating, gradually adding aluminum sulfate, zinc oxide, magnesium hydroxide and sodium fluoride, controlling the temperature at 60 ℃ and the stirring speed at 300 r/min; when the solution reached a milky white liquid (the solid was completely dissolved), the heating was stopped and the stirring was continued.
Step 3, when the temperature is reduced to 45 ℃, adding the betaine, and continuing stirring until the betaine is completely dissolved;
step 4, when the temperature is reduced to 35 ℃, adding a crystal inhibitor and a polycarboxylic acid high-performance water reducing agent, and stirring for 15min at a stirring speed of 550 r/min;
and 5, when the temperature is reduced to 30 ℃, adding the self-made biological enzyme, and continuously stirring for 10min to obtain a white emulsion finished product, namely the alkali-free liquid accelerator containing the biological enzyme.
Example 8
The preparation method of the alkali-free liquid accelerator containing the biological enzyme comprises the following steps:
step 1, adding tap water and aluminum hydroxide which account for half of the mass of the aluminum hydroxide into a container, starting a heating device, stirring into paste, gradually adding coordinated fluosilicic acid while stirring, controlling the speed of adding the fluosilicic acid to avoid boiling overflow, simultaneously adding phosphoric acid, controlling the heating temperature at 70 ℃, stopping heating, and controlling the stirring speed at 600r/min for 40min because the heat release temperature of the neutralization reaction can reach 90-100 ℃.
Step 2, adding the rest tap water, continuously stirring and heating, gradually adding aluminum sulfate, zinc oxide, magnesium hydroxide and sodium fluoride, controlling the temperature at 80 ℃ and the stirring speed at 500 r/min; when the solution reached a milky white liquid (the solid was completely dissolved), the heating was stopped and the stirring was continued.
Step 3, when the temperature is reduced to 50 ℃, adding the betaine, and continuing stirring until the betaine is completely dissolved;
step 4, when the temperature is reduced to 45 ℃, adding a crystal inhibitor and a polycarboxylic acid high-performance water reducing agent, and stirring for 20min at a stirring speed of 650 r/min;
and 5, when the temperature is reduced to 40 ℃, adding the self-made biological enzyme, and continuously stirring for 20min to obtain a white emulsion finished product, namely the alkali-free liquid accelerator containing the biological enzyme.
And preparing white emulsion according to the mass percentages of the components in the embodiments 1-5 and the synthesis method in the embodiment 6 respectively to obtain the alkali-free liquid accelerator containing the biological enzyme. When in use, the concrete is mixed with 5-9% of the cementing material according to the operating specification of sprayed concrete (the recommended mixing amount is 7%).
Examples 1 to 5 the following performances were obtained (accelerating agent for shotcrete GB/T35159-2017, content 7%)
Description of the drawings: the contents of chloride ions and fluoride ions are less than or equal to 0.05 percent, the 6h compressive strength is more than or equal to 1.0MPa, the 1d compressive strength is more than or equal to 10.0MPa, and the retention rate of the 90d compressive strength is more than or equal to 105 percent.
The data of the above examples 1-5 show that all indexes of the alkali-free liquid accelerator containing biological enzyme prepared by the invention meet the standards, and the alkali-free liquid accelerator is non-toxic and pollution-free, has high 1d compressive strength and good product placement stability, and can be seen that the coordinated fluosilicic acid is used for replacing the fluosilicic acid, so that the content of fluorine ions reaches the specification of the national iron enterprise standard (censorship).
As can be seen from the comparison of the data of examples 2 and 5, after the self-made biological enzyme is added, the stability of the material is improved, the net slurry setting time is shortened, and the strength of the mortar is improved. In addition, by adding the homemade biological enzyme, the sterilization and disinfection can be realized, and the physical health of operators can be protected.
Claims (3)
1. The alkali-free liquid accelerator containing the biological enzyme is characterized by comprising the following components in percentage by mass: fluosilicic acid: 16-20, aluminum hydroxide: 3-6, phosphoric acid: 0.1-0.2, aluminum sulfate: 38-42, zinc oxide: 0.02 to 0.07, magnesium hydroxide: 5-10, sodium fluoride: 0.1-0.4, betaine: 0.1-0.4, crystal inhibitor: 1-4, polycarboxylic acid high-performance water reducing agent: 0.04-0.07, self-made biological enzyme: 0.2-0.5, tap water: 18 to 37;
the homemade biological enzyme is prepared by the following method, and comprises the following components in percentage by mass: 30% of crushed and cleaned fruit and vegetable plants, 1% of liquorice, 0.5% of vitamin, 5% of brown sugar and 63.5% of tap water are placed in a clean container, the container is sealed and placed for 4-6 months at 15-30 ℃, and the obtained clear liquid is the self-made biological enzyme after filtration;
the fluosilicic acid is coordinated well by nano silicon dioxide; the specific coordination process of the fluorosilicic acid coordinated well through the nano-silica comprises the steps of adding the nano-silica into the fluorosilicic acid, stirring for 30min, standing for 24h, and taking a supernatant; the mass ratio of the nano silicon dioxide to the fluosilicic acid is 5-10: 100, respectively;
the crystal inhibitor is any one of acetone, ethanol and methanol.
2. The method for preparing the alkali-free liquid accelerator containing the biological enzyme according to claim 1, which is characterized by comprising the following steps of:
step 1, adding nano silicon dioxide into fluosilicic acid, stirring for 30min, standing for 24h, and taking clear liquid to obtain coordinated fluosilicic acid;
step 2, adding tap water and aluminum hydroxide into a container, stirring the mixture into paste at 50-70 ℃, then sequentially adding phosphoric acid and coordinated fluosilicic acid at the speed of 400-;
step 3, adding tap water, aluminum sulfate, zinc oxide, magnesium hydroxide and sodium fluoride at the temperature of 60-80 ℃ and the speed of 300-;
step 4, when the temperature is reduced to 45-50 ℃, adding betaine, and continuing stirring until the betaine is completely dissolved;
step 5, when the temperature is reduced to 35-45 ℃, adding a crystal inhibitor and a polycarboxylic acid high-performance water reducing agent, and stirring for 15-20min at the stirring speed of 550-650 r/min;
and 6, when the temperature is reduced to 30-40 ℃, adding the self-made biological enzyme, and continuously stirring for 10-20min to obtain a white emulsion finished product, namely the alkali-free liquid accelerator containing the biological enzyme.
3. The method of claim 2, wherein: in the step 1, the mass ratio of the nano silicon dioxide to the fluosilicic acid is 5-10: 100, respectively; in the step 2, the mass ratio of tap water to aluminum hydroxide is 1: 2; in the method, the mass ratio of total tap water, aluminum hydroxide, phosphoric acid, coordinated fluosilicic acid, aluminum sulfate, zinc oxide, magnesium hydroxide, sodium fluoride, betaine, a crystal inhibitor, a polycarboxylic acid high-performance water reducing agent and self-made biological enzyme used in steps 2 and 3 is 18-37: 3-6: 0.1-0.2: 16-20: 38-42: 0.02-0.07: 5-10: 0.1-0.4: 0.1-0.4: 1-4: 0.04-0.07: 0.2 to 0.5.
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