CN117368423A - Quality inspection method for geopolymer and application thereof - Google Patents
Quality inspection method for geopolymer and application thereof Download PDFInfo
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- 229920000876 geopolymer Polymers 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000007689 inspection Methods 0.000 title claims abstract description 15
- 239000007791 liquid phase Substances 0.000 claims description 40
- 239000010881 fly ash Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000012360 testing method Methods 0.000 claims description 17
- 239000007790 solid phase Substances 0.000 claims description 16
- 239000003518 caustics Substances 0.000 claims description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 14
- 239000011707 mineral Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000010802 sludge Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 12
- 229910052602 gypsum Inorganic materials 0.000 claims description 11
- 239000010440 gypsum Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 239000003513 alkali Substances 0.000 abstract description 19
- 238000001514 detection method Methods 0.000 abstract description 4
- 235000010755 mineral Nutrition 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000011575 calcium Substances 0.000 description 8
- 238000006703 hydration reaction Methods 0.000 description 8
- 239000004568 cement Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000004448 titration Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 241001411320 Eriogonum inflatum Species 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 235000011116 calcium hydroxide Nutrition 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- -1 alkali metal cations Chemical class 0.000 description 2
- 239000008231 carbon dioxide-free water Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000006174 pH buffer Substances 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 229910014472 Ca—O Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- GGCSIYPORILHKL-UHFFFAOYSA-L calcium;hydrogen carbonate;chloride Chemical compound Cl.[Ca+2].[O-]C([O-])=O GGCSIYPORILHKL-UHFFFAOYSA-L 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000012691 depolymerization reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910001653 ettringite Inorganic materials 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011413 geopolymer cement Substances 0.000 description 1
- 229920003041 geopolymer cement Polymers 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Processing Of Solid Wastes (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the field of geopolymer detection, and discloses a quality inspection method of a geopolymer and application thereof. The quality inspection method for the geopolymer provided by the invention is used for evaluating the alkali residue content in the geopolymer, so that the delivery quality of the geopolymer product can be ensured to reach the standard uniformly under the condition of maintaining higher production efficiency.
Description
Technical Field
The invention relates to the field of geopolymer detection, in particular to a quality inspection method of a geopolymer and application thereof.
Background
The geopolymer is an amorphous to semi-crystalline solid material formed by filling network gaps with alkali metal cations and alkaline earth metal cations, wherein the amorphous to semi-crystalline solid material is formed by connecting silicon oxygen tetrahedrons and aluminum oxygen tetrahedrons with angular peaks and has an irregular three-dimensional network structure. The geopolymer has wide sources of production raw materials, and solid wastes containing aluminosilicate series can be mostly used for preparing the geopolymer or geopolymer products. The geopolymer does not burn cement clinker, has very low energy consumption to produce it, but has superior properties to cement in many application environments. Geopolymers are considered green gelling materials that are likely to largely replace cement in the 21 st century. With the continuous maturity of mass production technology of geopolymer, the production cost of the geopolymer will be greatly reduced, the application technology will be more mature, and various excellent performances will be further developed. The popularization and application of geopolymers will lead to a number of new building material products to produce spanned changes in performance and cost.
The main component of the caustic sludge is Ca (OH) 2 The alkaline is higher, the comprehensive utilization rate is low, and serious pollution can be caused by long-term stacking. In order to solve the problem of excessive alkaline residue, the alkaline residue is utilized as a geopolymer alkaline excitant to provide a strong alkaline environment required by initial hydration for slag-fly ash composite cementing materials, and the slag materials firstly undergo hydration reaction and then Ca (OH) in a system 2 Further reacts with the fly ash to produce volcanic ash. Under the excitation of alkaline environment, the Ca-O bond of slag is weak, the calcium-rich phase is destroyed, and a large amount of Ca is dissolved out 2+ With OH - Combine to generate Ca (OH) with certain content 2 The method provides conditions for the pozzolan reaction of the fly ash, enhances the precipitation and the agglomeration of slag hydration gel products, accelerates the slag hydration process, and ensures that the two hydration reactions mutually restrict and complement each other, so that the mechanical strength of the geopolymer is greatly improved. And the caustic sludge with large mixing amount can cause compression strength collapse and adversely affect the development of mechanical properties in the later period of materials, so that the caustic sludge belongs to small mixing amount objects (0.1-3%) in raw materials for preparing geopolymer, and the problem of difficulty in uniform mixing in the production quality control of industrial project products is solved, and the quality control of product delivery is greatly affected.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, the uniformity of the content of alkaline residue in the production process of a geopolymer is difficult to control, and the delivery quality of a geopolymer product fluctuates greatly.
To achieve the above object, a first aspect of the present invention provides a quality inspection method of a geopolymer, comprising the steps of:
(1) Arbitrarily selecting x geopolymer samples from the geopolymer, wherein the weight of any one geopolymer sample is not less than 1g, and the mass ratio of each of the x geopolymer samples to water is 1:8-12, respectively obtaining x parts of a first liquid phase and x parts of a first solid phase after first solid-liquid separation, respectively testing the pH value of the x parts of the first liquid phase, and if the absolute value of the pH value difference between any two parts is more than or equal to 0.1, failing the geopolymer;
(2) If the absolute value of the pH value difference between any two parts of x parts of the first liquid phase is less than 0.1, the x parts of the first solid phase are respectively and independently mixed with water according to the mass ratio of 1:8-12, respectively obtaining x parts of a second liquid phase and x parts of a second solid phase after second solid-liquid separation, respectively testing the pH value of the x parts of the second liquid phase, and if the absolute value of the pH value difference value between any two parts of the x parts of the second liquid phase is less than 0.1, qualifying the geopolymer, otherwise, disqualifying the geopolymer;
wherein x is an integer not less than 2;
the geopolymer contains a component A and alkaline residue, and the pH value of the alkaline residue is higher than that of any one of the component A by more than 1.0.
A second aspect of the invention provides the use of a method for quality inspection of geopolymers as described in the first aspect above in the field of geopolymer production.
The quality inspection method of the geopolymer, provided by the invention, can be used for detecting whether the alkaline residue in the geopolymer is uniformly distributed in the production process more quickly, conveniently and intuitively, and if the alkaline residue is not uniformly distributed, the production technical parameters are timely adjusted, the real-time monitoring is carried out, and the timely feedback is given to the production. The quality inspection method for the geopolymer provided by the invention is used for evaluating the alkali residue content in the geopolymer, so that the delivery quality of the geopolymer product can be ensured to reach the standard uniformly under the condition of maintaining higher production efficiency.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the invention, the mass of the sample to be measured is measured to be accurate to a micrometer position; before the pH value of each sample to be tested is tested, the pH meter is required to be calibrated, the calibration method of the pH meter is not particularly limited, a person skilled in the art can select the pH meter according to the technical means known in the art, and exemplary pH buffers with pH values of 4.00 and 9.18 are prepared as the standard solutions, the temperature of the pH buffers is controlled to be 22±1 ℃, and the calibration is performed by adopting a two-point calibration method according to the instrument operation guidelines.
As described above, a first aspect of the present invention provides a method for quality inspection of a geopolymer, comprising the steps of:
(1) Arbitrarily selecting x geopolymer samples from the geopolymer, wherein the weight of any one geopolymer sample is not less than 1g, and the mass ratio of each of the x geopolymer samples to water is 1:8-12, respectively obtaining x parts of a first liquid phase and x parts of a first solid phase after first solid-liquid separation, respectively testing the pH value of the x parts of the first liquid phase, and if the absolute value of the pH value difference between any two parts is more than or equal to 0.1, failing the geopolymer;
(2) If the absolute value of the pH value difference between any two parts of x parts of the first liquid phase is less than 0.1, the x parts of the first solid phase are respectively and independently mixed with water according to the mass ratio of 1:8-12, respectively obtaining x parts of a second liquid phase and x parts of a second solid phase after second solid-liquid separation, respectively testing the pH value of the x parts of the second liquid phase, and if the absolute value of the pH value difference value between any two parts of the x parts of the second liquid phase is less than 0.1, qualifying the geopolymer, otherwise, disqualifying the geopolymer;
wherein x is an integer not less than 2;
the geopolymer contains a component A and alkaline residue, and the pH value of the alkaline residue is higher than that of any one of the component A by more than 1.0.
Preferably, the pH value of the alkaline residue is 1-1.5 higher than the component with the largest pH value in the component A. The inventor of the present invention found in the study that under the preferred conditions, the quality inspection method of the geopolymer provided by the present invention is more accurate and has better repeatability.
In the invention, the pH value of any one of the alkaline residue or the component A is detected by adopting the following method: accurately weighing 1g (up to 0.0001 g) of a sample to be tested into a centrifuge tube, and placing the sample into the centrifuge tube according to the following steps: deionized water is added in a mass ratio of water=1:10, the mixture is mixed for 1min at 100rpm, the mixture is put into a centrifuge and centrifuged for 5min at 4000rpm, the supernatant is taken out, the pH value is tested after the supernatant is filtered by filter paper, and the supernatant is read after the value is stable.
In the present invention, the water used in the measurement of the pH is preferably deionized water.
Preferably, x is an integer from 3 to 5.
Preferably, the time of the first mixing and the second mixing is each independently 1-2min.
More preferably, the conditions of the first mixing and the second mixing each independently satisfy: the shaking speed is 50-100rpm, and the time is 1-2min.
Preferably, the temperature of the first liquid phase and the second liquid phase is each independently 20-25 ℃.
The specific operations of the first solid-liquid separation and the second solid-liquid separation are not particularly limited, and may be selected by those skilled in the art according to technical means known in the art, and the operations of the first solid-liquid separation or the second solid-liquid separation include, for example: centrifuging at 4000-6000rpm for 5-10min, and filtering the supernatant with filter paper to obtain the first liquid phase or the second liquid phase.
Preferably, the component A is at least one selected from mineral powder, fly ash, gypsum and red mud.
According to a preferred embodiment, the geopolymer comprises, based on 100 parts by weight of the total weight of the geopolymer: 30-60 parts of mineral powder, 10-30 parts of fly ash, 10-30 parts of gypsum, 5-30 parts of red mud and 0.1-3 parts of caustic sludge.
More preferably, the geopolymer comprises, based on 100 parts by weight of the total weight of the geopolymer: 40-50 parts of mineral powder, 15-25 parts of fly ash, 15-25 parts of gypsum, 10-20 parts of red mud and 0.5-1.6 parts of caustic sludge.
Particularly preferably, the geopolymer comprises, based on 100 parts by weight of the total weight of the geopolymer: 40-50 parts of mineral powder, 15-25 parts of fly ash, 15-25 parts of gypsum, 10-20 parts of red mud and 0.5-1.3 parts of caustic sludge.
Preferably, ca (OH) in the alkaline residue 2 The content is 70 to 80wt%, more preferably 73 to 79wt%.
Preferably, the mineral powder is S95-grade granulated blast furnace slag powder meeting the requirements of GB/T18046-2000 standard.
Preferably, the red mud is sintered red mud.
Preferably, the fly ash is secondary fly ash meeting the GB/T1596-2005 standard requirements.
Preferably, the gypsum has a specific surface area of greater than 100m 2 /kg。
According to a preferred embodiment, the pH of the ore fines is 8.00-8.20, the pH of the fly ash is 8.90-9.10, the pH of the gypsum is 8.70-8.90, the pH of the red mud is 11.00-11.30, and the pH of the alkaline residue is 12.30-12.50.
As previously mentioned, a second aspect of the present invention provides the use of a method for mass inspection of geopolymers as described in the first aspect above in the field of geopolymer production.
The invention will be described in detail below by way of examples. In the examples below, all of the raw materials were commercially available, and the room temperature was 25.+ -. 2 ℃ unless otherwise specified.
In the following examples, pH was measured by a pH meter (manufacturer: shanghai electric instruments Co., ltd., model PHS-25) which was calibrated according to the instructions of instrument operation and the temperature of the solution to be measured was maintained at 22.+ -. 1 ℃.
Mineral powder: in order to meet the S95-grade granulated blast furnace slag powder required by GB/T18046-2000 standard, the pH value is 8.14;
fly ash: the pH value of the secondary fly ash is 9.03 in order to meet the requirements of GB/T1596-2005 standard;
gypsum: is dihydrate gypsum with specific surface area of 158m 2 Kg, pH 8.85;
red mud: the pH value of the sintered red mud is 11.18;
alkaline residue: ca (OH) 2 The content was 78.07wt% and the pH was 12.44.
Test example 1
(1) Preparing 10kg of geopolymers with different alkaline residue contents according to the formula of table 1, numbering the prepared geopolymers as a sample 1 to a sample 13 in sequence according to the trend of increasing the alkaline residue content, fully and uniformly mixing all components in the geopolymers, weighing 1g (accurate to 0.0001 g) of the sample 1 to the sample 13 respectively, placing the samples into a centrifuge tube respectively, and placing the samples into the centrifuge tube according to the following steps: adding deionized water into the water with the mass ratio of water=1:10, mixing for 1min at 100rpm, putting into a centrifuge, centrifuging at 4000rpm for 5min, taking out to obtain a first solid phase sinking at the bottom of the centrifuge tube, filtering the supernatant with filter paper to obtain first liquid phases of samples 1 to 13 respectively, measuring the pH value of the first liquid phase by a pH meter, reading after the value is stable, repeating the test for 3 times, and taking an average value;
(2) The absolute value of the difference value of the pH values of the first liquid phases of two adjacent samples from the sample 5 to the sample 9 is less than 0.1, and the samples of the part are selected to carry out the following operations:
adding deionized water into each centrifuge tube filled with the first solid phase according to the mass ratio of 1:10, adopting the mixing and solid-liquid separation operation same as that of the step (1) to obtain a second solid phase and a second liquid phase, adopting a pH meter to measure the pH value of the second liquid phase, reading after the value is stable, repeating the test for 3 times, and taking an average value.
The pH results of each sample are shown in Table 1.
TABLE 1
As can be seen from the data in Table 1, the pH of the first liquid phase is 10.65 when the caustic sludge content in the geopolymer is 0wt%, and the pH of the system reaches 11.37 when 0.3wt% caustic sludge is added, indicating that caustic sludge is the main source of alkalinity for the system. When the alkali slag content is 1.0-1.6wt%, the pH value of the system gradually rises, but the change is relatively small, and when the alkali slag content is 1.8-3.0wt%, the pH value of the system reaches more than 12.00.
It is known that when the pH of the test geopolymer is lower than 11.82, the alkali residue accounts for less than 1.0wt% of the raw material, and when the pH of the test geopolymer is higher than 12.07, the alkali residue accounts for more than 1.8wt% of the raw material, and the approximate proportion of the alkali residue in the raw material can be primarily judged according to the test pH. And (3) adding water into the first solid phase of samples 5 to 9 of which the absolute value of the pH value difference of the first liquid phase of two adjacent samples is less than 0.1, wherein after the pH value of the obtained second liquid phase is tested, the pH value of the second liquid phase is in the range of 10.60-11.33, and the absolute value of the pH value difference between the samples is more than or equal to 0.1.
That is, the alkaline residue is a main alkaline source of a geopolymer system, and the uniformity of the alkaline residue content at different positions can be judged by sampling and testing the pH values at different positions of the geopolymer in the production process. The absolute value of the pH value difference of the second liquid phase of the sampled sample at different positions of the geopolymer is controlled to be less than 0.1, so that the alkaline residue content error at different positions of the geopolymer in the production process is controlled to be within +/-0.1 wt%, the yield of the factory quality of the geopolymer product is greatly improved, and the quality inspection method of the geopolymer provided by the invention is simpler, more convenient and faster, can give timely feedback to production, and maintains higher production efficiency.
Test example 2
The compressive strength of each geopolymer sample prepared in example 1 was tested and the results are shown in table 2.
TABLE 2
According to the regulations of GB 175-2007 general Portland Cement and Q/GPM 001-2023, the compressive strength requirements of the geopolymer 425 cement are shown in Table 2, that is, in Table 2, the standard refers to the standard compressive strength of the geopolymer 425 cement, and the geopolymer 425 cement refers to the common geopolymer cement with the 28-day standard mortar compressive strength of not less than 42.5 MPa.
As can be seen from the data in Table 2, when the sample with the alkali residue content of 0wt% (sample 1) in the geopolymer shows no strength at early stage, the strengths of 7d and 28d are also lower, namely, only 6.3MPa and 30.1MPa, and the alkali residue is used as an alkali excitant to provide alkali environment required for initial hydration for the mineral powder-fly ash composite cementing material, so that the activities of mineral powder and fly ash are excited, the activation and decomposition of the mineral powder-fly ash vitreous granules are promoted, and the depolymerization reaction occurs, if the alkali residue in the system is not used, the mineral powder-fly ash hydration reaction can not be hardly excited only by the alkalinity of red mud, and only weak hydration reaction can occur on the surface of the material. When 0.3wt% caustic sludge (sample 2) was added, the sample started to have strength early, but was still low, and the 1d and 3d strengths were only 0.3MPa and 8.6MPa, which did not meet the standard. With the increase of the alkali residue content (0.5-1.3 wt%), namely samples 3-6, the 3d and 28d strength of the geopolymer samples can meet the standard specification requirements, wherein the 3d strength of the sample with the alkali residue content of 1.0wt% (sample 5) reaches 26.8MPa, and the 28d strength with the alkali residue content of 0.5wt% (sample 3) reaches 49.7MPa. However, when the alkali slag content (1.4-3.0 wt%) was further increased, i.e., samples 7-13, the strength of the samples decreased with the increase in the alkali slag content, wherein the strength of samples 3d, 28d having an alkali slag content of 3.0% (sample 13) was only 10.1MPa, 14.5MPa, which is also because too high alkali content affected the ettringite morphology formed by the system, causing expansion destruction, which was detrimental to the strength of the cement. From the viewpoint of combining early and later strength performance, the acceptable blending amount of the caustic sludge in the geopolymer ranges from 0.5 to 1.3wt%. The specific existing content of the alkaline residue can be further judged according to the pH value test result, and the production quality is regulated and controlled.
The preferable geopolymer composition formula provided by the invention can enable the geopolymer product to have more excellent compressive strength.
Example 1
The formulation shown in sample 6 was expanded to add the components in the geopolymer to 1000 kg. The geopolymer quality was evaluated according to the following quality test method.
In the production process, 3 different parts (named as A part, B part and C part) of the geopolymer are sampled, 1g (0.0001 g accurate) of each sample of A, B, C part is weighed, respectively named as A-1, B-1 and C-1, and are respectively and independently mixed with water according to the mass ratio of 1:10 (100 rpm and 1 min), and a first liquid phase and a first solid phase are respectively obtained after first solid-liquid separation (4000 rpm and 5 min), and the pH value of the first liquid phase is respectively tested;
the first solid phases were each independently mixed with water (100 rpm,1 min) in a mass ratio of 1:10, and after the second solid-liquid separation (4000 rpm,5 min), a second liquid phase and a second solid phase were each obtained, and the pH of the second liquid phase was each tested.
Repeating the test twice again, weighing 1g (0.0001 g) of each sample of A, B, C parts, and respectively named A-2, B-2 and C-2; each sample of A, B, C parts (accurate to 0.0001 g) was weighed and designated A-3, B-3 and C-3, respectively. The pH values of the first liquid phase and the second liquid phase are respectively tested according to the operation, and the repeatability verification is carried out on the method.
And the calcium hydroxide content in each part sample and the alkaline residue is tested by adopting a calcium sucrose-hydrochloric acid titration method, so that the accuracy of the method is verified.
Calcium sucrose-hydrochloric acid titration method:
(1) 1g of sample (m, accurate to 0.0001 g) was weighed, placed in a 250mL dry conical flask, 50mL of carbon dioxide-free water was quickly added, the flask was quickly capped, the conical flask was shaken to disperse the sample, the flask was opened, 25mL of boiling water was added, the flask was shaken, quickly heated to boil for 1min, the conical flask was removed, the flask was loosely capped, and the flask was cooled to room temperature in a cold water bath.
(2) Adding 50mL sucrose solution, covering the bottle stopper, shaking, standing for 5min, shaking every 5min during this period, removing the bottle stopper, and flushing the bottle stopper and bottle wall with carbon dioxide free water. Adding 6-7 drops of phenolphthalein indicator solution, titrating with hydrochloric acid standard titration solution, adding 1 drop of titration speed per second at the near end point, and continuously shaking the conical flask until the pink color of the solution disappears, and adding the last drop of hydrochloric acid standard solution until no pink color appears within 30s (V). The test flow of the method is more than or equal to 30 minutes.
Wherein:
W Ca(OH)2 -mass fraction of available calcium hydroxide, wt%;
T Ca(OH)2 titre of hydrochloric acid standard titration solution to calcium hydroxide in milligrams per milliliter (mg/mL)；
V-the volume of hydrochloric acid standard titration solution is consumed in milliliters (mL) during titration;
mthe mass of the sample is given in grams (g).
The content of calcium hydroxide in the alkaline residue is 78.07wt% by the method, and the content of the alkaline residue in the sample 6 is determined by the method as follows:
wherein:
W-determining the content of alkaline residue in sample 6, wt%;
W 1 -determining the content of calcium hydroxide in sample 6, wt%;
W 2 -measuring hydrogen in alkaline residueCalcium oxide content, wt%.
The results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the data in Table 3, the pH results of several groups of samples 6 at 3 different locations of the geopolymer were consistent with the methodology of the present invention, while the detection data for the amount of caustic sludge in sample 6 was about 1.3wt% by calcium gluconate-hydrochloric acid titration, both methods being able to determine the presence of caustic sludge in the geopolymer.
Compared with a calcium carbonate-hydrochloric acid titration method or other chemical titration analysis methods, the quality evaluation method for the geopolymer product provided by the invention has good repeatability and accuracy, can be used for detecting whether the alkaline residue in the geopolymer is uniformly distributed in the production process more quickly, conveniently and intuitively, can control the whole detection process within 15min, monitors the existence content of the alkaline residue of the geopolymer in real time, gives timely feedback to the production, and has high efficiency.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A method for quality inspection of a geopolymer, comprising the steps of:
(1) Arbitrarily selecting x geopolymer samples from the geopolymer, wherein the weight of any one geopolymer sample is not less than 1g, and the mass ratio of each of the x geopolymer samples to water is 1:8-12, respectively obtaining x parts of a first liquid phase and x parts of a first solid phase after first solid-liquid separation, respectively testing the pH value of the x parts of the first liquid phase, and if the absolute value of the pH value difference between any two parts is more than or equal to 0.1, failing the geopolymer;
(2) If the absolute value of the pH value difference between any two parts of x parts of the first liquid phase is less than 0.1, the x parts of the first solid phase are respectively and independently mixed with water according to the mass ratio of 1:8-12, respectively obtaining x parts of a second liquid phase and x parts of a second solid phase after second solid-liquid separation, respectively testing the pH value of the x parts of the second liquid phase, and if the absolute value of the pH value difference value between any two parts of the x parts of the second liquid phase is less than 0.1, qualifying the geopolymer, otherwise, disqualifying the geopolymer;
wherein x is an integer not less than 2;
the geopolymer contains a component A and alkaline residue, and the pH value of the alkaline residue is higher than that of any one of the component A by more than 1.0.
2. The method of claim 1, wherein x is an integer from 3 to 5.
3. The method according to claim 1 or 2, wherein the time of the first mixing and the second mixing is each independently 1-2min.
4. The method according to claim 1 or 2, wherein the temperature of the first liquid phase and the second liquid phase is each independently 20-25 ℃.
5. The method according to claim 1 or 2, wherein the component a is selected from at least one of mineral powder, fly ash, gypsum, red mud.
6. The method according to claim 5, wherein the geopolymer comprises, based on 100 parts by weight of the total weight of the geopolymer: 30-60 parts of mineral powder, 10-30 parts of fly ash, 10-30 parts of gypsum, 5-30 parts of red mud and 0.1-3 parts of caustic sludge.
7. The method according to claim 1 or 2, characterized in that Ca (OH) in the alkaline residue 2 The content is 70-80wt%.
8. The method according to claim 5, wherein the mineral powder is S95-grade granulated blast furnace slag powder meeting the requirements of GB/T18046-2000 standard; and/or the number of the groups of groups,
the red mud is sintered red mud.
9. The method according to claim 5, wherein the pH value of the mineral powder is 8.00-8.20, the pH value of the fly ash is 8.90-9.10, the pH value of the gypsum is 8.70-8.90, the pH value of the red mud is 11.00-11.30, and the pH value of the alkaline residue is 12.30-12.50.
10. Use of a method for quality inspection of geopolymers according to any one of claims 1 to 9 in the field of geopolymer preparation.
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