CN109796141B - Sulfur-fixing ash geopolymer and preparation method thereof - Google Patents
Sulfur-fixing ash geopolymer and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a sulfur-fixing ash geopolymer, which comprises the following steps: A) carrying out steam treatment on the sulfur fixation ash powder; B) mixing the solid sulfur ash powder obtained in the step A) with alkali metal hydroxide and alkali metal salt to obtain a powder mixture; C) and mixing the powder mixture with water, adding an alkaline activator, forming, and maintaining to obtain the sulfur-fixing ash geopolymer. The application also provides a sulfur fixation ash geopolymer. In the process of preparing the sulfur-fixing ash geopolymer, the application prolongs the setting time of the geopolymer and improves the compressive strength of the geopolymer by modifying the sulfur-fixing ash and changing the feeding mode.
Description
Technical Field
The invention relates to the technical field of building material manufacturing, in particular to a sulfur-fixing lime geopolymer and a preparation method thereof.
Background
The sulfur-fixing ash is a by-product generated after coal is combusted in the circulating fluidized bed boiler, the combustion temperature of the circulating fluidized bed boiler is lower than that of a four-corner tangential boiler (about 900 ℃), limestone is required to be added as a sulfur-fixing agent in the combustion process, and if the combustion operation control is not good, the sulfur-fixing ash is high in free calcium oxide, high in ignition loss and contains unreacted CaCO3In addition, the reaction product CaSO of the in-furnace desulfurization is also contained4Different from the spherical microstructure of common fly ash,the surface structure of the sulfur-fixing ash particles is loose and irregular, and the common microstructure is shown in figure 1. The common sulfur-fixing ash mineral comprises amorphous phase, free calcium oxide and unreacted CaCO3、CaSO4And quartz crystal phase, and the XRD spectrum is shown in figure 2.
Geopolymers (geopolymers) are amorphous to semi-crystalline three-dimensional aluminosilicate polymeric materials in which the silicon and aluminum atoms within the material are connected by bridging oxygen atoms to form robust chemical bonds (Si-O-Al) metal cations (Na)+、K+、Ca2+) Filled in the grid gaps and has a structure and a composition similar to zeolite. The geopolymer is mainly reacted with a silicon-aluminum raw material through an alkaline activator, wherein the commonly used alkaline activator is selected from alkali metal hydroxide, alkali metal water glass and a mixture of the alkali metal hydroxide and the alkali metal water glass, and the commonly used silicon-aluminum raw material is selected from metakaolin, pumicite, fly ash, mineral waste residues, calcined clay and the like.
Studies have shown that the addition of calcium-rich substances to geopolymer systems reduces the setting time, which is associated with the production of a large number of additional heterogeneous coagulation nuclei in the system during the initial stages of the reaction, mainly due to Ca (OH)2The precipitate binds with the silicate gel around it. The different forms of the calcium-containing substances have different effects on the above-mentioned reactions, such as calcium substances in the form of calcium silicate salts and calcium aluminosilicates, free calcium oxide, calcium hydroxide, calcium sulfate, calcium carbonate, etc., which have a much shorter setting time than free calcium oxide and calcium hydroxide, which react with water in the system to form Ca (OH)2The consumption of water in the system limits the dissolution of the active silica-alumina in the fly ash, the reduction of the silica-alumina monomer in the solution, the reduction of the formation of geopolymer colloid, which leads to the reduction of the compressive strength of the geopolymer, and Ca (OH)2The content is high, only a small part of the content is converted into a CSH gelled phase which can increase the compressive strength, so the compressive strength is reduced due to the high content; calcium materials in the form of calcium silicate salts and calcium aluminosilicates can participate in the reaction to form calcium silicate hydrate (C-S-H) and calcium aluminate hydrate (C-A-H) gel phases which can improve the compressive strength of the material, but when the system alkalinity is relatively high (above 10M), precipitates can be formed without other reverse reactionsShould occur or as a secondary product. Therefore, it is of great significance and difficulty to extend the setting time of geopolymers and ensure higher compressive strength.
Disclosure of Invention
The invention aims to provide a preparation method of a sulfur-fixing ash geopolymer, and the sulfur-fixing ash geopolymer provided by the application can prolong the solidification time of the geopolymer and has higher compressive strength.
In view of the above, the present application provides a method for preparing a sulfur-fixing ash geopolymer, comprising the following steps:
A) carrying out steam treatment on the sulfur fixation ash powder;
B) mixing the solid sulfur ash powder obtained in the step A) with alkali metal hydroxide and alkali metal salt to obtain a powder mixture;
C) and mixing the powder mixture with water, adding an alkaline activator, forming, and maintaining to obtain the sulfur-fixing ash geopolymer.
Preferably, the alkali activator is prepared from alkali metal hydroxide and alkali metal water glass.
Preferably, the content of the sulfur-fixing ash is 100 parts by weight, the content of the alkaline hydroxide is 2-10 parts by weight, the content of the alkali metal salt is 0-3 parts by weight, and the content of the water is 8-30 parts by weight; in the alkali activator, the content of the alkali metal hydroxide is 2-10 parts by weight, and the content of the alkali metal water glass is 48-80 parts by weight.
Preferably, the modulus of the alkali-activator is 0.88 to 2.2.
Preferably, the fineness of the sulfur fixation ash is below 45 mu m and the screen residue is not more than 12%.
Preferably, the modulus of the alkali metal water glass is 2.2-3.4, and the baume degree is 40 or 50.
Preferably, the alkali metal salt is selected from one or more of alkali metal sulfate, alkali metal phosphate and alkali metal carbonate.
Preferably, the alkali-activator is placed for 24-48 h before use.
The application also provides a sulfur fixation ash geopolymer which is prepared from a powder material and a liquid material; the powder material comprises sulfur fixation ash, alkali metal hydroxide and alkali metal salt, and the liquid material comprises water and an alkaline activator.
Preferably, the content of the sulfur-fixing ash is 100 parts by weight, the content of the alkaline hydroxide is 2-10 parts by weight, the content of the alkali metal salt is 0-3 parts by weight, and the content of the water is 8-30 parts by weight; the alkali activator is prepared from 2-10 parts by weight of alkali metal hydroxide and 48-80 parts by weight of alkali metal water glass.
The application provides a preparation method of a solid sulfur ash geopolymer, which comprises the steps of firstly treating solid sulfur ash powder by steam to convert free calcium oxide in the solid sulfur ash into calcium hydroxide, then mixing and grinding the solid sulfur ash subjected to steam treatment, alkali metal hydroxide and alkali metal salt, promoting depolymerization of silicon and aluminum in the solid sulfur ash by the introduced alkali metal hydroxide, promoting dissolution of silicon and aluminum substances, reacting the introduced alkali metal salt with calcium hydroxide to generate calcium salt and alkali metal hydroxide, and promoting dissolution of the silicon and aluminum substances again; the mixing mode of firstly adding water and then adding the alkaline exciting agent plays a role in promoting the dissolution of the silicon-aluminum substances and then the polymerization, so that the solidification time is prolonged, and the precipitation of the silicon-aluminum substances is beneficial to improving the compressive strength of the sulfur-fixing lime geopolymer.
Drawings
FIG. 1 is an SEM photomicrograph of a prior art solid sulfur ash of the present invention;
FIG. 2 is an XRD spectrum of a sulfur fixation ash in the prior art;
FIG. 3 is a schematic flow diagram of the preparation of a sulfur-fixing ash geopolymer according to an embodiment of the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the technical problems that the preparation setting time of the solid sulfur ash geopolymer in the prior art is short and the compressive strength cannot be considered, the application aims to reduce the content of calcium substances such as free calcium oxide, calcium hydroxide and the like which are unfavorable for strength in the solid sulfur ash, promote the dissolution of active silicon and aluminum in the solid sulfur ash, solve the problem that the solid sulfur ash is unfavorable for casting molding when being rapidly solidified in the preparation of the geopolymer, and simultaneously improve the compressive strength of the geopolymer. Therefore, the preparation method of the sulfur-fixing ash geopolymer is beneficial to dissolving out silicon-aluminum substances and can delay the setting time of the sulfur-fixing ash geopolymer.
The embodiment of the invention discloses a preparation method of a sulfur-fixing ash geopolymer, which specifically comprises the following steps of:
A) carrying out steam treatment on the sulfur fixation ash powder;
B) mixing the solid sulfur ash powder obtained in the step A) with alkali metal hydroxide and alkali metal salt to obtain a powder mixture;
C) and mixing the powder mixture with water, adding an alkaline activator, forming, and maintaining to obtain the sulfur-fixing ash geopolymer.
In the process of preparing the solid sulfur ash geopolymer, the solid sulfur ash powder is firstly modified, namely, the solid sulfur ash powder is firstly subjected to steam treatment, so that free calcium oxide in the solid sulfur ash is converted into calcium hydroxide. The solid sulfur ash powder is well known to those skilled in the art, and the source of the solid sulfur ash powder is not particularly limited in the present application, and in the present application, the fineness of the solid sulfur ash powder is 45 μm or less and the screen residue is not more than 12%. The specific mode of operation of the steam treatment is not particularly limited in this application and is a mode well known to those skilled in the art; and the steam treatment time is 20-40 min, and after the steam treatment is finished, the sulfur fixation ash is placed in a drying box for cooling.
According to the invention, the sulfur-fixing ash is mixed with alkali metal hydroxide and alkali metal salts after being treated by steam to complete the modification of the sulfur-fixing ash; in this process, the alkali metal hydroxide promotes depolymerization of silico-aluminum in the sulfur-fixing ash to promote dissolution of silico-aluminum substances, and the alkali metal salt reacts with the generated calcium hydroxide to generate a calcium salt and an alkali metal hydroxide to promote dissolution of silico-aluminum substances again. The alkali metal in the above-mentioned alkali metal hydroxide may be selected from Na or K, and the alkali metal salt is a commercially available product and may be selected from one or more of alkali metal sulfate, alkali metal phosphate and alkali metal carbonate, and in specific examples, the alkali metal salt is selected from alkali metal sulfate, and more specifically, the alkali metal salt is selected from sodium sulfate. After the mixing, placing the obtained mixture in a 105 ℃ oven for more than 4 hours to obtain a powder mixture.
And mixing the obtained powder mixture with water, stirring for 60 seconds, adding an alkaline activator, stirring for 2min, casting, molding and maintaining to obtain the sulfur-fixing ash geopolymer. In the process, water is added to promote the silicon and aluminum substances in the sulfur-fixing ash to be dissolved out as much as possible, and an alkaline activator is added to delay the coagulation time. In the above process, the modulus of the alkali-activator is 0.88 to 2.2, and in specific embodiments, the modulus of the alkali-activator is 1.0 to 1.8. The alkali activator is prepared from alkali metal hydroxide and alkali metal water glass, wherein the alkali metal water glass is a commercially available product, the modulus is 2.2-3.4, and the Baume degree is 40 or 50.
In the process of preparing the sulfur-fixing ash geopolymer, the dosage of all the raw materials is as follows: 100 parts of sulfur-fixing ash, 2-10 parts of alkali metal hydroxide, 0-3 parts of alkali metal salt, 8-30 parts of water, 2-10 parts of alkali metal hydroxide in an alkaline activator and 48-80 parts of alkali metal water glass. The dosage of the alkali metal hydroxide added in the modification of the sulfur fixation ash is 30 to 60 percent of the total alkali consumption.
In the process of preparing the solid sulfur ash geopolymer, the coagulation time of the solid sulfur ash geopolymer is prolonged and the compressive strength of the geopolymer is improved by means of modifying the solid sulfur ash, changing the feeding mode and the like.
The application also provides a sulfur fixation ash geopolymer which is prepared from a powder material and a liquid material; the powder material comprises sulfur fixation ash, alkali metal hydroxide and alkali metal salt, and the liquid material comprises water and an alkaline activator.
The above-mentioned sulfur-fixing ash, alkali metal hydroxide, alkali metal salt and alkali activator have been described in detail, and are not described in detail herein.
For the sulfur-fixing ash geopolymer, the content of the sulfur-fixing ash is 100 parts by weight, the content of the alkaline hydroxide is 2-10 parts by weight, the content of the alkali metal salt is 0-3 parts by weight, and the content of the water is 8-30 parts by weight; the alkali activator is prepared from 2-10 parts by weight of alkali metal hydroxide and 48-80 parts by weight of alkali metal water glass.
For further understanding of the present invention, the following examples are provided to illustrate the preparation of the sulfur-fixing lime geopolymer of the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
The embodiment is a preparation method of a high-calcium sulfur-fixing ash geopolymer for prolonging the setting time, which specifically comprises the following steps:
(1) liquid alkaline activator preparation
Preparing an alkali metal hydroxide aqueous solution: 4.2 parts by weight of 96 percent purity NaOH is dissolved and added with 53.3 parts by weight of alkali metal sodium silicate to be mixed, and the mixture is placed for 24 hours;
(2) modification of sulfur fixation ash
Passing hot steam into 100 parts by weight of high-calcium sulfur fixation ash for 30min, and then placing the high-calcium sulfur fixation ash in a drying oven to cool the high-calcium sulfur fixation ash to room temperature; grinding the high-calcium sulfur fixation ash, 6.5 parts by weight of alkali metal hydroxide and 2 parts by weight of sodium sulfate together, and then placing the mixture in a 105 ℃ oven for 4 hours;
(3) solid-liquid mixing forming
Firstly, adding 16 parts by weight of water into the powder material, stirring for 1min, adding the prepared alkaline excitation liquid, stirring for 2min to form slurry, and pouring and forming to obtain the sulfur-fixing lime geopolymer.
The test sample is sealed and then is placed in a 60 ℃ oven for maintenance, the depth of the Vicat needle penetrating into the sample is measured every 2min, when the penetration depth of the needle is 25mm, the initial setting time is recorded, when the penetration depth of the needle is 0mm, the final setting time is recorded, and the test results are shown in Table 1; the results show that: the compressive strength of the sulfur-fixing lime geopolymer 28d prepared in the example is 42.14MPa, the initial setting time is 37min, and the final setting time is 69 min.
Example 2
The embodiment is a production method of a high-calcium sulfur-fixing ash geopolymer capable of prolonging the setting time, which specifically comprises the following steps:
(1) liquid alkaline activator preparation
Preparing an alkali metal hydroxide aqueous solution: 5.3 parts by weight of 96 percent purity NaOH is dissolved and added with 66.7 parts by weight of alkali metal sodium silicate to be mixed, and the mixture is placed for 24 hours;
(2) modification of sulfur fixation ash
Passing hot steam through 100 parts by weight of high-calcium sulfur fixation ash for 30min, then placing the high-calcium sulfur fixation ash in a drying oven to cool to room temperature, grinding the high-calcium sulfur fixation ash together with 3.0 parts by weight of alkali metal hydroxide and 2 parts by weight of sodium sulfate, and then placing the ground high-calcium sulfur fixation ash in a 105 ℃ drying oven for 4 hours;
(3) solid-liquid mixing forming
Firstly, adding 25 parts by weight of water into a powder material, stirring for 1min, adding the prepared alkaline excitation liquid, stirring for 2min to form slurry, and pouring and forming to obtain the sulfur-fixing lime geopolymer.
The test sample is sealed and then is placed in a 60 ℃ oven for maintenance, the depth of the Vicat needle penetrating into the sample is measured every 2min, when the penetration depth of the needle is 25mm, the initial setting time is recorded, when the penetration depth of the needle is 0mm, the final setting time is recorded, and the test results are shown in Table 1; the results show that: the compressive strength of the sulfur-fixing lime geopolymer 28d prepared in the example is 39.72MPa, the initial setting time is 49min, and the final setting time is 78 min.
Example 3
The embodiment is a production method of a high-calcium sulfur-fixing ash geopolymer capable of prolonging the setting time, which specifically comprises the following steps:
(1) liquid alkaline activator preparation
Preparing an alkali metal hydroxide aqueous solution: 4.2 parts by weight of 96 percent purity NaOH is dissolved and added with 53.3 parts by weight of alkali metal sodium silicate to be mixed, and the mixture is placed for 24 hours;
(2) modification of sulfur fixation ash
Passing hot steam through 100 parts by weight of high-calcium sulfur fixation ash for 30min, then placing the high-calcium sulfur fixation ash in a drying oven to cool to room temperature, grinding the high-calcium sulfur fixation ash together with 6.5 parts by weight of alkali metal hydroxide and 2 parts by weight of sodium sulfate, and then placing the ground high-calcium sulfur fixation ash in a 105 ℃ drying oven for 4 hours;
(3) solid-liquid mixing forming
Firstly, adding 30 parts by weight of water into a powder material, stirring for 1min, adding the prepared alkaline excitation liquid, stirring for 2min to form slurry, and pouring and forming to obtain the sulfur-fixing lime geopolymer.
The test sample is sealed and then is placed in a 60 ℃ oven for maintenance, the depth of the Vicat needle penetrating into the sample is measured every 2min, when the penetration depth of the needle is 25mm, the initial setting time is recorded, when the penetration depth of the needle is 0mm, the final setting time is recorded, and the test results are shown in Table 1; the results show that: the compressive strength of the sulfur-fixing lime geopolymer 28d prepared in the example is 40.08MPa, the initial setting time is 57min, and the final setting time is 89 min.
Comparative example 1
The comparative example is a production method of a traditional sulfur fixation ash geopolymer, and specifically comprises the following steps:
(1) liquid alkaline activator preparation
Preparing an alkali metal hydroxide aqueous solution: 10.7 parts by weight of 96% pure NaOH is dissolved in 16 parts by weight of water, mixed with 53.3 parts by weight of alkali metal sodium silicate and placed for 24 hours;
(2) solid-liquid mixing forming
And mixing the prepared liquid alkaline exciting agent with 100 parts by weight of unmodified high-calcium sulfur fixation ash, stirring for 3min to form slurry, and pouring and forming to obtain the sulfur fixation ash geopolymer.
The test sample is sealed and then is placed in a 60 ℃ oven for maintenance, the depth of the Vicat needle penetrating into the sample is measured every 2min, when the penetration depth of the needle is 25mm, the initial setting time is recorded, when the penetration depth of the needle is 0mm, the final setting time is recorded, and the test results are shown in Table 1; the results show that: the compressive strength of the sulfur-fixing lime geopolymer 28d prepared by the comparative example is 31.45MPa, the initial setting time is 7min, and the final setting time is 23 min.
Comparative example 2
The comparative example is a production method of a traditional sulfur fixation ash geopolymer, and specifically comprises the following steps:
(1) liquid alkaline activator preparation
Preparing an alkali metal hydroxide aqueous solution: 8.3 parts by weight of 96% pure NaOH are dissolved in 25 parts by weight of water, mixed with 66.7 parts by weight of alkali metal sodium silicate and placed for 24 hours;
(2) solid-liquid mixing forming
And mixing the prepared liquid alkaline exciting agent with 100 parts by weight of unmodified high-calcium sulfur fixation ash, stirring for 3min to form slurry, and pouring and forming to obtain the sulfur fixation ash geopolymer.
The test sample is sealed and then is placed in a 60 ℃ oven for maintenance, the depth of the Vicat needle penetrating into the sample is measured every 2min, when the penetration depth of the needle is 25mm, the initial setting time is recorded, when the penetration depth of the needle is 0mm, the final setting time is recorded, and the test results are shown in Table 1; the results show that: the compressive strength of the sulfur-fixing lime geopolymer 28d prepared by the comparative example is 24.72MPa, the initial setting time is 17min, and the final setting time is 45 min.
Table 1 table of performance data for geopolymers prepared in examples and comparative examples
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A preparation method of a sulfur-fixing ash geopolymer comprises the following steps:
A) carrying out steam treatment on the sulfur fixation ash powder;
B) grinding the solid sulfur ash powder obtained in the step A) together with alkali metal hydroxide and alkali metal salt to obtain a powder mixture;
C) mixing the powder mixture with water, adding an alkaline activator, forming and maintaining to obtain a sulfur-fixing ash geopolymer;
the alkali activator is prepared from alkali metal hydroxide and alkali metal water glass;
the content of the sulfur fixation ash is 100 parts by weight, the content of the alkali metal hydroxide is 2-10 parts by weight, the content of the alkali metal salt is 0-3 parts by weight, and the content of the water is 8-30 parts by weight; in the alkaline activator, the content of the alkali metal hydroxide is 2-10 parts by weight, and the content of the alkali metal water glass is 48-80 parts by weight;
the fineness of the sulfur fixation ash powder is below 45 mu m and the screen residue is not more than 12%.
2. The production method according to claim 1, wherein the modulus of the alkali-activator is 0.88 to 2.2.
3. The method according to claim 1, wherein the alkali water glass has a modulus of 2.2 to 3.4 and a baume degree of 40 or 50.
4. The method according to claim 1, wherein the alkali metal salt is one or more selected from the group consisting of an alkali metal sulfate, an alkali metal phosphate and an alkali metal carbonate.
5. The preparation method according to claim 1, wherein the alkali-activator is left for 24 to 48 hours before use.
6. The sulfur-fixing ash geopolymer prepared by the preparation method of claim 1, which is prepared from a powder material and a liquid material; the powder material comprises sulfur fixation ash, alkali metal hydroxide and alkali metal salts, and the liquid material comprises water and an alkaline activator; the alkali activator is prepared from alkali metal hydroxide and alkali metal water glass;
the content of the sulfur fixation ash is 100 parts by weight, the content of the alkali metal hydroxide is 2-10 parts by weight, the content of the alkali metal salt is 0-3 parts by weight, and the content of the water is 8-30 parts by weight; the alkali activator is prepared from 2-10 parts by weight of alkali metal hydroxide and 48-80 parts by weight of alkali metal water glass.
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