CN112624643A - Preparation method of optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer - Google Patents
Preparation method of optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer Download PDFInfo
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- CN112624643A CN112624643A CN202011570187.0A CN202011570187A CN112624643A CN 112624643 A CN112624643 A CN 112624643A CN 202011570187 A CN202011570187 A CN 202011570187A CN 112624643 A CN112624643 A CN 112624643A
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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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
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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
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
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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
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
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- 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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- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Treatment Of Sludge (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a preparation method of an optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer, which adopts the technical scheme that the preparation method comprises the following steps: carrying out synergistic wet grinding on 90-200 parts of phosphorus slag and 50-100 parts of nickel slag according to the water-material ratio of 0.3-0.7 until the median particle size is 1-4 mu m to obtain slurry A; crushing the optical fiber waste mud, and sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder; wet grinding the optical fiber dry powder according to the water-material ratio of 0.3-0.7 until the median particle size is 100-800nm to obtain slurry B; taking 120 parts of slurry A, 35 parts of optical fiber waste mud dry powder, 5-50 parts of slurry B, 10-40 parts of phosphogypsum, 20-50 parts of carbide slag and 20-50 parts of Na2CO3Mixing and stirring the materials in a colloid-sand ratio of 1: 3 preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer by using a mortar stirrer. The invention has simple operation and greatly reduces the production costThe method solves the problems of land occupation and environmental pollution caused by solid waste stacking, and has higher economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a preparation method of an optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer.
Background
With the development of economy, environmental problems become increasingly serious. Yellow phosphorus has rapidly increased in yield year by year over the last 10 years. But a large amount of industrial waste residue, namely phosphorus slag, can be produced while producing yellow phosphorus. The phosphorus slag has low utilization rate, is piled in the open air all the year round, occupies land, and the phosphorus and fluorine in the phosphorus slag are gradually dissolved out by rainwater and permeate underground, so that water sources are polluted, plant growth is influenced, and human health is harmed. A great deal of financial and energy is spent on treating environmental pollution treatment and related social problems every year.
With the increasing increase of the environmental pollution problem caused by climate warming, the environmental protection consciousness is raised, and the requirements and the demands of people on green environment-friendly materials are increased day by day. The alkali-activated cementing material is a low-carbon cementing material taking silicon-aluminum waste as a raw material. Because of the advantages of low energy consumption, less emission, high strength, good durability and the like, the material is consistently considered as a green cementing material with wide application prospect by many researchers.
The geopolymer is a novel green building material, takes industrial solid wastes with wide sources as raw materials, has low energy consumption, low carbon emission, convenient preparation, excellent compressive and flexural strength, acid and alkali corrosion resistance, freeze thawing resistance and carbonization resistance, has wide application prospect, and is one of the best substitutes of common portland cement-based materials.
The waste optical fiber mud is one kind of industrial waste effluent exhausted during the industrial production process in producing prefabricated rod and other photoelectronic products. At present, most of waste mud is treated as waste by a landfill method. However, the landfill method not only occupies precious land resources, but also easily causes serious problems of ecological damage, environmental pollution and the like.
Patent CN105693118A discloses a method for preparing an alkali-activated phosphorus slag-based cementing material with adjustable conductivity. The material comprises the following components: the phosphorus slag, the carbon ash, the sodium silicate nonahydrate and the potassium hydroxide are mixed by a stirring device, and the conductive alkali-activated phosphorus slag-based semiconductor cementing material is obtained through die forming and curing.
Patent CN201810851330.X specifically discloses a geopolymer concrete and a preparation method thereof, and the material components comprise: mineral powder, fly ash, silica fume, a composite excitant, a water reducer, a retarder and the like, and the method provides a new way for the high-efficiency resource application of the high-aluminum-content alkaline waste liquid generated in the processing process of the aluminum alloy raw material. But strong alkali is used for excitation, which is not beneficial to popularization.
Disclosure of Invention
The invention aims to provide a preparation method of an optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer, which has the advantages of simple process, low cost and low energy consumption.
The invention provides a preparation method of an optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer, which comprises the following steps:
(1) feeding 90-200 parts of phosphorus slag, 50-100 parts of nickel slag and 75-125 parts of water into a planetary ball mill according to the water-material ratio of 0.3-0.7 for wet grinding until the median particle size is 1-4 mu m to obtain slurry A, wherein the phosphorus slag is waste obtained by calcining at 1350-1400 ℃ in the preparation process of yellow phosphorus, and the phosphorus slag mainly comprises CaO and SiO2The nickel slag is granulated slag formed by naturally cooling or water quenching a melt formed in the nickel metal smelting process, and mainly comprises FeO and SiO2、Al2O3And MgO;
(2) crushing the optical fiber waste mud, and sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder;
(3) putting 150-0.7 parts of dry powder of the waste optical fiber mud and 75-125 parts of water into a planetary ball mill according to the water-material ratio of 0.3-0.7, and grinding the mixture to 800nm to obtain slurry B, wherein the waste optical fiber mud is waste material in the process of manufacturing optical fibers and mainly comprises SiO2；
120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 5-50 parts of slurry B obtained in the step (3), 10-40 parts of phosphogypsum, 20-50 parts of carbide slag and 20-50 parts of Na2CO3Mixing and stirring the materials in a colloid-sand ratio of 1: 3 preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer by using a mortar stirrer.
The phosphorus slag is waste obtained by calcining at 1350-1400 ℃ in the preparation process of yellow phosphorus, and the nickel slag is granulated slag formed by naturally cooling or water quenching a melt formed in the nickel metal smelting process; and putting the phosphorus slag and the nickel slag into a planetary ball mill together to grind for 40-60min until the median particle size is 1-4 mu m.
And crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
And (3) putting the dry powder of the optical fiber waste mud into a planetary ball mill for grinding for 40-60min until the median particle size is 100-800 nm.
The phosphogypsum is anhydrous phosphogypsum calcined at 500 ℃.
The carbide slag is industrial waste slag generated when acetylene is obtained by hydrolyzing carbide.
Na2CO3Is anhydrous sodium carbonate.
The rotating speed of the planetary ball mill in the step is 100-400 rad/s.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention relates to a wet grinding process, which utilizes the gelled material which is subjected to wet grinding and has high efficiency and low energy consumption to be subjected to superfine treatment, ions are easy to dissolve out, the hydration speed is higher, and the activity is higher. Avoids the dry grinding process with high energy consumption and solves the problem that fine particles are easy to agglomerate.
The invention takes phosphorus slag, phosphogypsum, optical fiber waste mud, alkaline industrial waste residue carbide slag and the like as raw materials and takes P dissolved out by ions after wet grinding3-And alkaline industrial residue Ca2+And OH-Reaction to generate hydroxyapatite Na2CO3The hydroxyapatite can be further carbonized to form carbonized hydroxyapatite, the strength is further improved, the hydroxyapatite has stable structure and strong adsorption capacity. Meanwhile, hydroxyapatite can be used as a crystal nucleus to induce the precipitation of cement hydration products and promote the reaction.
The particle size of the wet-milled fiber waste mud can reach 100-800nm, the wet-milled fiber waste mud can be used as a nano material, has the characteristics of better induced hydration, early strength promotion and no side effect, has a nanocrystal core effect, and ensures that the hydration environment is in an alkaline state after wet milling. The optical fiber waste mud crystal nucleus has heterogeneous nucleation characteristics, the formation of dihydrate gypsum can be promoted, the early strength is improved, and as time goes on, when the nano material is hydrated, a hydration product is preferentially hydrated on the nano crystal nucleus to generate calcium silicate hydrate gel, so that the later strength is improved.
The nickel slag which is wet-milled in the invention is used as a partial cementing material and is subjected to cooperative wet milling with the phosphorous slag, so that the fineness of the phosphorous slag can be reduced, the surface activity is improved, and the nickel slag can provide an aluminum phase and a silicon phase in the reaction process so as to react to generate calcium silicate hydrate gel and ettringite and improve the strength.
The dry powder of the non-wet-milled optical fiber waste mud is used as a partial cementing material, so that the compactness of a test block can be improved, the pores can be reduced, and the strength can be improved.
The invention provides a full-solid waste green invention process, and simultaneously reduces the production cost of calcium silicate hydrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following further provides embodiments and examples of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration only. In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The specific implementation mode of the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer is as follows:
example 1
(1) And (3) feeding 140 parts of phosphorus slag, 60 parts of nickel slag and 100 parts of water into a planetary ball mill according to the water-material ratio of 0.5 for grinding for 40min at the rotating speed of the planetary ball mill of 100 plus 400rad/s to obtain the slurry A.
(2) Crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
(3) 200 parts of optical fiber waste mud dry powder and 100 parts of water are sent into a planetary ball mill according to the water-material ratio of 0.5 for wet grinding, the grinding time is 40min, and the rotating speed of the planetary ball mill is 400rad/s, so that slurry B is obtained.
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 5 parts of slurry B obtained in the step (3), 20 parts of phosphogypsum, 45 parts of carbide slag and Na2CO3And uniformly mixing and stirring 38.5 parts of sand and 900 parts of sand, and stirring and forming to obtain the mortar test block. The mechanical property of the mixture is tested by reference to the standard GB8076-2008, and the mixture is tested at the humidity of more than 90 percent and the temperature of 20 +/-1 DEG CThe standard curing room is maintained for 3d, 7d and 28d, and the measured strength of the mortar test block is shown in table 1.
Example 2
(1) And (2) feeding 140 parts of phosphorus slag, 60 parts of nickel slag and 100 parts of water into a planetary ball mill according to the water-material ratio of 0.5 for grinding for 40min at the rotating speed of the planetary ball mill of 400rad/s to obtain slurry A.
(2) Crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
(3) 200 parts of optical fiber waste mud dry powder and 100 parts of water are sent into a planetary ball mill according to the water-material ratio of 0.5 for wet grinding, the grinding time is 40min, and the rotating speed of the planetary ball mill is 400rad/s, so that slurry B is obtained.
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 15 parts of slurry B obtained in the step (3), 20 parts of phosphogypsum, 45 parts of carbide slag, Na2CO3And uniformly mixing and stirring 38.5 parts of sand and 900 parts of sand, and stirring and forming to obtain the mortar test block. The mechanical property of the mixture is tested according to the reference standard GB8076-2008, the mixture is maintained for 3d, 7d and 28d in a standard maintenance room with the humidity of more than 90% and the temperature of 20 +/-1 ℃, and the strength of the tested mortar test block is shown in Table 1.
Example 3
(1) And (2) feeding 140 parts of phosphorus slag, 60 parts of nickel slag and 100 parts of water into a planetary ball mill according to the water-material ratio of 0.5 for grinding for 40min at the rotating speed of the planetary ball mill of 400rad/s to obtain slurry A.
(2) Crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
(3) 200 parts of optical fiber waste mud dry powder and 100 parts of water are sent into a planetary ball mill according to the water-material ratio of 0.5 for wet grinding, the grinding time is 40min, and the rotating speed of the planetary ball mill is 400rad/s, so that slurry B is obtained.
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 25 parts of slurry B obtained in the step (3), 20 parts of phosphogypsum, 45 parts of carbide slag and Na2CO3And uniformly mixing and stirring 38.5 parts of sand and 900 parts of sand, and stirring and forming to obtain the mortar test block. Reference standard GB8076-2008 stirringAnd (3) performing mechanical property test on the compound, curing the compound in a standard curing room with the humidity of more than 90% and the temperature of 20 +/-1 ℃ for 3d, 7d and 28d, and obtaining the strength of the mortar test block shown in the table 1.
Example 4
(1) And (2) feeding 140 parts of phosphorus slag, 60 parts of nickel slag and 100 parts of water into a planetary ball mill according to the water-material ratio of 0.5 for grinding for 40min at the rotating speed of the planetary ball mill of 400rad/s to obtain slurry A.
(2) Crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
(3) 200 parts of optical fiber waste mud dry powder and 100 parts of water are sent into a planetary ball mill according to the water-material ratio of 0.5 for wet grinding, the grinding time is 40min, and the rotating speed of the planetary ball mill is 400rad/s, so that slurry B is obtained.
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 35 parts of slurry B obtained in the step (3), 20 parts of phosphogypsum, 45 parts of carbide slag and Na2CO3And uniformly mixing and stirring 38.5 parts of sand and 900 parts of sand, and stirring and forming to obtain the mortar test block. The mechanical property of the mixture is tested according to the reference standard GB8076-2008, the mixture is maintained for 3d, 7d and 28d in a standard maintenance room with the humidity of more than 90% and the temperature of 20 +/-1 ℃, and the strength of the tested mortar test block is shown in Table 1.
Example 5
(1) And (2) feeding 140 parts of phosphorus slag, 60 parts of nickel slag and 100 parts of water into a planetary ball mill according to the water-material ratio of 0.5 for grinding for 40min at the rotating speed of the planetary ball mill of 400rad/s to obtain slurry A.
(2) Crushing the optical fiber waste mud, and then sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder.
(3) 200 parts of optical fiber waste mud dry powder and 100 parts of water are sent into a planetary ball mill according to the water-material ratio of 0.5 for wet grinding, the grinding time is 40min, and the rotating speed of the planetary ball mill is 400rad/s, so that slurry B is obtained.
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 50 parts of slurry B obtained in the step (3), 20 parts of phosphogypsum, 45 parts of carbide slag and Na2CO338.5 parts of sand and 900 parts of sand are uniformly mixed and stirredStirring and molding to obtain the mortar test block. The mechanical property of the mixture is tested according to the reference standard GB8076-2008, the mixture is maintained for 3d, 7d and 28d in a standard maintenance room with the humidity of more than 90% and the temperature of 20 +/-1 ℃, and the strength of the tested mortar test block is shown in Table 1.
Comparative example 1
Comparative example 1 is a mortar blank without any activator, and the measured mortar test block strength is shown in table 1.
Comparative example 2
Comparative example 2 is a mortar control group to which only the carbide slag was added, and the strength of the mortar test block is shown in table 1.
Comparative example 3
Comparative example 3A mortar control group of carbide slag and sodium carbonate was added, and the strength of the mortar test block is shown in Table 1.
Comparative example 4
Comparative example 4 mortar control without addition of the fiber slurry, the mortar test block strength measured is shown in table 1.
TABLE 1 mortar test Block Strength measured in the examples
As can be seen from Table 1, the strength of the geopolymer consisting of only slurry A and phosphogypsum is very low, but with carbide slag and Na2CO3The strength is increased to a certain extent by being mixed with exciting agents such as dry fiber powder and the like, but the strength per day is increased by 250% with the mixing of the slurry B, the effect is extremely remarkable, the strength is increased more with the increase of the mixing amount, the mixing amount of 7% is the optimal mixing amount, and the strength is slightly reduced with the mixing amount of more than 7%.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the invention, and the invention is intended to cover modifications, equivalents, and improvements within the spirit and scope of the present invention.
Claims (10)
1. A preparation method of an optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer comprises the following steps:
(1) feeding 90-200 parts of phosphorus slag, 50-100 parts of nickel slag and 75-125 parts of water into a planetary ball mill according to the water-material ratio of 0.3-0.7, and carrying out wet grinding until the median particle size is 1-4 mu m to obtain slurry A;
(2) crushing the optical fiber waste mud, and sieving the crushed optical fiber waste mud by a 1.18mm sieve to obtain optical fiber waste mud dry powder;
(3) sending 150-250 parts of dry powder of the waste fiber mud and 75-125 parts of water into a planetary ball mill according to the water-material ratio of 0.3-0.7 to grind to 800nm to obtain slurry B;
(4) 120 parts of slurry A obtained in the step (1), 35 parts of dry powder of the fiber waste mud obtained in the step (2), 5-50 parts of slurry B obtained in the step (3), 10-40 parts of phosphogypsum, 20-50 parts of carbide slag and 20-50 parts of Na2CO3Mixing and stirring the materials in a colloid-sand ratio of 1: 3 preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer by using a mortar stirrer.
2. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 1, the phosphorous slag is waste obtained by calcining at 1350-1400 ℃ in the preparation process of yellow phosphorus, and the main components of the phosphorous slag are CaO and SiO2The nickel slag is granulated slag formed by naturally cooling or water quenching a melt formed in the nickel metal smelting process, and mainly comprises FeO and SiO2、Al2O3And MgO.
3. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 1, the phosphorous slag and the nickel slag are put into a planetary ball mill to be ground for 40-60min in a synergic manner, and the ground particles have a median particle size of 1-4 μm.
4. The method of claim 1, wherein the SiO in the optical fiber is SiO in the optical fiber2The content is more than 90 percent.
5. The method for preparing the optical fiber waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 2, the optical fiber waste mud is crushed and then passes through a 1.18mm screen to obtain the optical fiber waste mud dry powder.
6. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 3, the optical fiber waste mud dry powder is put into a planetary ball mill for grinding for 40-60min, and the particle size is 100-800 nm.
7. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 4, the phosphogypsum is anhydrous phosphogypsum calcined at 500 ℃.
8. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 4, the carbide slag is industrial waste slag generated when acetylene is obtained by hydrolyzing carbide.
9. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in claim 1, wherein in the step 4, the Na is added2CO3Is anhydrous sodium carbonate.
10. The method for preparing the optical fiber-doped waste mud alkali-activated phosphorous slag geopolymer as claimed in any one of claims 1 to 9, wherein the rotation speed of the planetary ball mill in the step 3 is 100-400 rad/s.
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