CN110526631B - Fly ash-based geopolymer material for solidifying chromium slag and preparation method thereof - Google Patents
Fly ash-based geopolymer material for solidifying chromium slag and preparation method thereof Download PDFInfo
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- CN110526631B CN110526631B CN201910878895.1A CN201910878895A CN110526631B CN 110526631 B CN110526631 B CN 110526631B CN 201910878895 A CN201910878895 A CN 201910878895A CN 110526631 B CN110526631 B CN 110526631B
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- 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
Abstract
The invention relates to a fly ash-based polymer material for curing chromium slag and a preparation method thereof, wherein the fly ash-based polymer is prepared from the following raw materials in parts by mass: 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary portland cement, 15-20 parts of water, 0.1-0.3 part of water reducer, 0.1-0.3 part of modified PVA (polyvinyl alcohol) fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag. The compression strength of the solidified fly ash geopolymer of the invention after being solidified for 7 days is over 30MPa, which is far more than 7MPa required by national standard GB14569.1-93 solidified body performance requirements of low and medium level radioactive waste, and the hexavalent chromium leaching concentration of the solidified fly ash geopolymer is less than 1mg/L and far less than 5mg/L specified in GB5085.3-2007 identification Standard for hazardous substances and identification of leaching toxicity.
Description
Technical Field
The invention relates to the technical field of geopolymer-based materials, in particular to a fly ash-based polymer material for solidifying chromium slag and a preparation method thereof.
Background
The chromium slag is industrial solid waste produced in the process of producing metal chromium and chromium salt in the metallurgical department and chemical industry, and is solid waste residue remained after adding limestone, dolomite, sodium carbonate and the like into chromite, roasting at the high temperature of 1200 ℃ with 1000-plus-materials, and leaching out soluble salt in the chromite by using water. In the production of chromium salt in China, 2-3t of chromium slag is discharged when 1t of chromium salt is produced, about 7t of chromium slag is discharged when 1t of metal chromium is produced, the chromium slag discharged by China is about 20 ten thousand tons as a large country for producing chromium salt, and the amount of the chromium slag stockpiled in all years is over 300 ten thousand tons. The accumulation of the chromium slag not only occupies a large amount of land, but also can seriously pollute soil and water sources if the water-soluble and acid-soluble hexavalent chromium leached after being leached by rainwater enters the water sources without being treated and discharged at will, thereby harming human bodies. The geopolymer is an inorganic high polymer with a three-dimensional network structure of a silicon-oxygen tetrahedron and an aluminum-oxygen tetrahedron, which is prepared by taking natural minerals or solid wastes and artificially synthesized silicon-aluminum materials as raw materials and activating at normal temperature through alkali, has good curing capability, high mechanical property, excellent chemical corrosion resistance, high temperature resistance and the like, and can be widely applied to the fields of communication facilities, airport runways, roads and bridges and the like. However, due to the selection of the types and amounts of the alkali-activator and the mineral, the selection of the geopolymer material still has the disadvantages of poor toughness, low curing strength, poor flowability, etc.
Disclosure of Invention
The invention aims to provide a fly ash-based polymer material for curing chromium slag and a preparation method thereof.
In order to achieve the above object, the present invention provides, in one aspect, a fly ash-based geopolymer material for solidifying chromium slag, characterized in that: the adhesive comprises the following components in parts by mass: 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary portland cement, 15-20 parts of water, 0.1-0.3 part of water reducer, 0.1-0.3 part of modified PVA (polyvinyl alcohol) fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag.
Preferably, the compound alkali activator is sodium silicate with initial modulus of 3-4 and solid content of 40% -60%, and sodium hydroxide solution is adopted to prepare sodium silicate with modulus of 0.8-1.6, and then the mixture is aged for 12-72 h;
the fly ash is high-calcium fly ash, wherein the content of calcium oxide is 10-20%;
firstly, ball milling the slag for 6-24 hours by using a ball mill by using a screening method so that the average grain diameter is 0.075-0.095 mm;
ball-milling the silicon powder by using a ball mill to ensure that the average particle size is 150-200 nm;
the calcined metakaolin was prepared as follows: calcining kaolin at 600-800 ℃ for 6-8 hours, then grinding and sieving to obtain the kaolin, wherein the average particle size of the kaolin is 100-150 nm;
the water reducing agent is sodium carbonate powder, and the content of the water reducing agent is 0.1-0.3% of the total composition;
the modified PVA fiber is a silane coupling agent modified PVA fiber, and the length of the modified PVA fiber is 3mm-6 mm; the modified PVA fiber is modified by the following steps: putting PVA fiber in absolute ethyl alcohol in KH560 silane coupling agent with the mass solubility of 9-11%, then oscillating for 2-4min by ultrasonic waves, and then washing and drying;
the length of the multi-wall carbon nano-tube is 3-12um, and the specific surface area is 233-2/g；
The solid content of the styrene-acrylic emulsion is 46-48%, and the viscosity is 200-800 Pa.s.
The invention also provides a preparation method of the fly ash-based geopolymer material for solidifying chromium slag, which is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary silicate cement, 15-20 parts of water, 0.1-0.3 part of water reducer, 0.1-0.3 part of modified PVA (polyvinyl alcohol) modified fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag;
(2) grinding and mixing calcined metakaolin, slag, silicon powder, fly ash, ordinary portland cement, a water reducing agent and chromium slag to obtain a mixture;
(3) and (2) placing the modified PVA fiber and the multi-walled carbon nano tube into a composite alkali-activated solution, oscillating for 2-4min by using ultrasonic waves, mixing with the mixture, and then adding water and a styrene-acrylic emulsion to obtain the fly ash-based polymer.
The fly ash-based geopolymer material for curing chromium slag and the traditional curing material have the following advantages:
(1) the fly ash based polymer material for curing the chromium slag adopts industrial waste residues, fly ash and other wastes, and can solve the environmental problem of waste slag pile.
(2) The fly ash based polymer material for curing the chromium slag can reduce the cost and lead the solid waste to be recycled.
(3) The fly ash-based polymer material for curing the chromium slag has the advantages of good flowing property, high early-stage cured body strength, good metal ion curing property, good durability and the like.
(4) Compared with the traditional process, the preparation method of the fly ash-based polymer material for curing chromium slag is simple and easy to popularize.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The present invention is further illustrated in detail below with reference to specific examples.
In the following embodiments, the fly ash based geopolymer material for curing the chromium slag comprises the following components in parts by mass: the raw materials for preparing the material comprise the following components in parts by mass: 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary portland cement, 15-20 parts of water, 0.1-0.3 part of water reducer, 0.1-0.3 part of modified PVA (polyvinyl alcohol) fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag.
In the following embodiments, the dosage parts of each substance are parts by mass, and the composite alkali activator used in the following embodiments is composed of NaOH and an aqueous solution of Na2SiO3 with a solid content of 50%; the calcined metakaolin had an average particle size of 150 nm; the content of CaO in the high-calcium fly ash is 15 percent; the average particle size of the slag is 75 nm; the average grain diameter of the silica fume is 175 nm; it is characterized in that the content of the compound is 0.1 to 0.3 percent of the total composition; the solid content of the styrene-acrylic emulsion is 47%, and the viscosity is 600 Pa.s; the modified PVA fiber is prepared by the following method: putting PVA fiber into absolute ethyl alcohol in 10% KH560 silane coupling agent by mass, then oscillating for 3mins by ultrasonic wave, and then washing and drying; the length of the multi-wall carbon nano-tube is 6-8um, and the specific surface area is 240m2(ii)/g; the Portland cement is 42.5R ordinary Portland cement.
Example 1
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 25 parts of fly ash, 18 parts of chromium slag, 4 parts of slag, 4.5 parts of calcined metakaolin, 5 parts of silicon powder, 4 parts of 42.5R ordinary portland cement and 0.2 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.2 part of PVA fiber and 0.3 part of multi-walled carbon nano tube, stirring for 3min, adding 17.5 parts of water and 1.5 parts of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Example 2
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 25 parts of fly ash, 18 parts of chromium slag, 3 parts of slag, 5 parts of calcined metakaolin, 5 parts of silicon powder, 3.5 parts of 42.5R ordinary portland cement and 0.2 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.2 part of PVA fiber and 0.3 part of multi-walled carbon nano tube, stirring for 3min, adding 17.5 parts of water and 1.5 parts of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Example 3
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 22 parts of fly ash, 18.5 parts of chromium slag, 4 parts of slag, 4.5 parts of calcined metakaolin, 5 parts of silicon powder, 4 parts of 42.5R ordinary portland cement and 0.2 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.2 part of PVA fiber and 0.3 part of multi-wall carbon nano tube, stirring for 3min, adding 20 parts of water and 1.5 parts of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Example 4
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 25 parts of fly ash, 18 parts of chromium slag, 4 parts of slag, 4.5 parts of calcined metakaolin, 5 parts of silicon powder, 4 parts of 42.5R ordinary portland cement and 0.2 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.1 part of PVA fiber and 0.4 part of multi-wall carbon nano tube, stirring for 3min, adding 17.5 parts of water and 1.5 parts of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Example 5
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 25 parts of fly ash, 19 parts of chromium slag, 4 parts of slag, 4.5 parts of calcined metakaolin, 5 parts of silicon powder, 3 parts of 42.5R ordinary portland cement and 0.2 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.2 part of PVA fiber and 0.25 part of multi-wall carbon nano tube, stirring for 3min, adding 17.5 parts of water and 2 parts of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Example 6
The embodiment provides a geopolymer material for curing chromium slag fly ash, which comprises the following specific preparation methods: grinding 25 parts of fly ash, 18 parts of chromium slag, 4 parts of slag, 4.5 parts of calcined metakaolin, 5 parts of silicon powder, 4 parts of 42.5R ordinary portland cement and 0.1 part of water reducing agent in a planetary ball mill for 30min to obtain a premix for later use; adding premix into a cement paste mixer, adding 20 parts of composite alkali activator which is subjected to ultrasonic oscillation and comprises 0.2 part of PVA fiber and 0.4 part of multi-walled carbon nano tube, stirring for 3min, adding 18 parts of water and 1 part of styrene-acrylic emulsion, and stirring for 5min to obtain the cement paste.
Test example
The fly ash geopolymer materials for curing chromium slag prepared in examples 1 to 6 were subjected to performance tests using national standards for cement concrete/mortar, JGJ70-2009, JTGE30-2005, GB/T50081-2002, GB/T15555.4-1995, HJ/T299-2007 and GB5085.3-2007, the test results of which are shown in Table 1, wherein the setting time was measured according to JGJ70-2009, the fluidity was measured according to JTGE30-2005, the compressive strength was measured according to GB/T50081-2002, the leaching solubility of chromium ions was measured according to GB/T15555.4-1995, HJ/T299-2007 and GB5085.3-2007, and the leaching solubility of chromium ions was measured according to GB/T15555.4-1995, HJ/T299-2007 and GB5085.3-2007
Table 1 shows the results of the measurements of the properties of the fly ash geopolymer for curing chromium ions
While embodiments of the present invention have been described above, the above description is intended to be exemplary, not exhaustive, and not limited to any embodiments carelessly. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (2)
1. A fly ash based polymer material for solidifying chromium slag is characterized in that: the composition comprises the following components in parts by mass: 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary portland cement, 15-20 parts of water, 0.1-0.3 part of water reducing agent, 0.1-0.3 part of modified PVA fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag;
the compound alkali activator adopts sodium silicate with initial modulus of 3-4 and solid content of 40-60%, and adopts sodium hydroxide solution to prepare the sodium silicate with modulus of 0.8-1.6, and then the sodium silicate is aged for 12-72 h;
the fly ash is high-calcium fly ash, wherein the content of calcium oxide is 10-20%;
firstly, ball-milling the slag for 6-24 hours by using a screening ball mill to ensure that the average grain diameter is 0.075-0.095 mm;
ball-milling the silicon powder by using a ball mill to ensure that the average particle size is 150-200 nm;
the calcined metakaolin was prepared as follows: calcining kaolin at 600-800 ℃ for 6-8 hours, then grinding and sieving to obtain the metakaolin, wherein the average particle size of the metakaolin is 100-150 nm;
the water reducing agent is sodium carbonate powder, and the content of the water reducing agent is 0.1-0.3% of the total composition;
the modified PVA fiber is a silane coupling agent modified PVA fiber, and the length of the modified PVA fiber is 3mm-6 mm; the modified PVA fiber is modified by the following steps: putting the PVA fiber into absolute ethyl alcohol containing a KH560 silane coupling agent with the mass concentration of 9-11%, then oscillating for 2-4min by using ultrasonic waves, and then washing and drying;
the length of the multi-wall carbon nano-tube is 3-12um, and the specific surface area is 233-2/g；
The solid content of the styrene-acrylic emulsion is 46-48%, and the viscosity is 200-800 Pa.s.
2. A method of preparing a fly ash based geopolymer material for solidifying chromium slag according to claim 1, characterized in that: the method comprises the following steps:
(1) weighing 15-25 parts of composite alkali activator, 15-25 parts of fly ash, 3-5 parts of slag, 3-6 parts of calcined metakaolin, 4-6 parts of silicon powder, 3-5 parts of ordinary portland cement, 15-20 parts of water, 0.1-0.3 part of water reducing agent, 0.1-0.3 part of modified PVA fiber, 0.2-0.4 part of multi-walled carbon nanotube, 1-2 parts of styrene-acrylic emulsion and 17-19 parts of chromium slag;
(2) grinding and mixing calcined metakaolin, slag, silicon powder, fly ash, ordinary portland cement, a water reducing agent and chromium slag to obtain a mixture;
(3) and (2) placing the modified PVA fiber and the multi-walled carbon nano tube into a composite alkali-activated solution, oscillating for 2-4min by using ultrasonic waves, mixing with the mixture, and then adding water and a styrene-acrylic emulsion to obtain the fly ash-based polymer.
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| CN111689708B (en) * | 2020-05-07 | 2022-06-24 | 中国工程物理研究院材料研究所 | High-calcium geological cement for nuclide solidification and application method |
| CN111995309B (en) * | 2020-08-31 | 2022-01-04 | 武汉大学 | Geopolymer for marine concrete outer protective layer and preparation method thereof |
| CN111995308B (en) * | 2020-08-31 | 2022-03-04 | 武汉大学 | Ultrahigh-toughness multi-wall carbon nanotube-polyvinyl alcohol fiber modified geopolymer and preparation method thereof |
| CN112723801B (en) * | 2021-01-13 | 2022-06-03 | 武汉大学 | Cement concrete pavement rapid repairing material and preparation method thereof |
| CN113061019B (en) * | 2021-04-16 | 2022-07-01 | 山西太钢工程技术有限公司 | Method for preparing shaped brick from chromic acid-containing mud through low-temperature drying modification of rotary kiln |
| CN113501684A (en) * | 2021-07-22 | 2021-10-15 | 武汉大学 | Light high-ductility geopolymer material and preparation method thereof |
| CN113620626A (en) * | 2021-09-07 | 2021-11-09 | 中科镁基（北京）科技有限公司 | Method for preparing geopolymer by using chromium slag |
| CN115159882A (en) * | 2022-08-01 | 2022-10-11 | 江西理工大学 | Preparation process of rare earth waste residue geopolymer |
| CN116376331A (en) * | 2023-03-24 | 2023-07-04 | 辽宁省交通规划设计院有限责任公司 | Geopolymer-based inorganic reflective coating as well as preparation method and application thereof |
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