A high-performance microcrystalline glass based on multi-source solid waste and its preparation method

By preparing high-performance microcrystalline glass, using solid wastes such as oil-based rock debris degreasing residue and phosphorus slag as raw materials, the problem of their disposal and resource utilization has been solved, realizing high-value utilization and high-performance microcrystalline glass production.

CN119638200BActive Publication Date: 2026-01-30SOUTHWEST PETROLEUM UNIV
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Patent Information

Application Number
CN202411766362.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-04
Publication Date
2026-01-30
Estimated Expiration
2044-12-04

AI Technical Summary

Technical Problem

Existing technologies are insufficient for the effective disposal and resource utilization of solid wastes such as oil-based rock cuttings deoiling residues and phosphorus slag, resulting in limited resource utilization pathways.

Method used

High-performance microcrystalline glass was prepared by using oil-based rock debris deoiling residue and phosphorus slag as raw materials, combined with fly ash, and adjusting the MgO content. CAS-based and CMAS-based microcrystalline glass were prepared by using steps such as melting, water quenching, and ball milling.

Benefits of technology

This technology enables the high-value utilization of oil-based rock cuttings deoiling residue and phosphorus slag, producing high-performance microcrystalline glass that meets the "Industrial Microcrystalline Sheet" standard, while also reducing sintering temperature and cost.

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Abstract

This invention discloses a high-performance microcrystalline glass based on multi-source solid waste and its preparation method. The preparation method includes the following steps: S1: Obtaining oil-based rock cuttings degreasing residue and phosphorus slag, and respectively crushing, drying, ball milling, and sieving them to obtain residue powder and phosphorus slag powder; S2: Performing component analysis on the phosphorus slag powder to confirm the MgO content; according to the analysis results, mixing the residue powder and phosphorus slag powder with fly ash, and melting the mixture after uniform mixing to obtain a base glass melt; S3: Water quenching the base glass melt to obtain base glass, and then drying, ball milling, and sieving it to obtain base glass powder; S4: Forming the base glass powder into a microcrystalline glass prototype, sintering the microcrystalline glass prototype, and naturally cooling it to obtain high-performance microcrystalline glass. This invention can synergistically prepare high-performance microcrystalline glass from two types of solid waste: oil-based rock cuttings degreasing residue and phosphorus slag, realizing the synergistic high-value utilization of multi-source solid waste.
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Description

Technical Field

[0001] This invention relates to the field of collaborative high-value utilization technology of multi-source solid waste, and in particular to a high-performance microcrystalline glass based on multi-source solid waste and its preparation method. Background Technology

[0002] As solid waste generated from horizontal drilling using oil-based mud, oil-based rock cuttings have an oil content as high as 15-25%, falling under the category of "HW08 Waste Mineral Oil" in the National Hazardous Waste List. Pyrolysis technology treats oil-based rock cuttings under high-temperature thermal desorption conditions in an oxygen-deficient or oxygen-free environment, reducing the oil content to below 1%. While pyrolysis technology solves the problem of mineral oil recovery from oil-based rock cuttings, the disposal of the deoiled residue remains an issue. Traditionally, deoiled residue from oil-based rock cuttings is mainly used to prepare sintered bricks and cement, but the low product value hinders the willingness to utilize it, resulting in limited resource recovery pathways.

[0003] In addition, phosphorus slag is an industrial solid waste generated during the phosphorus chemical production process, mainly derived from the production of yellow phosphorus. Approximately 8-10 tons of phosphorus slag are generated for every 1 ton of yellow phosphorus produced. my country's annual phosphorus slag production exceeds 7 million tons, while the utilization rate is less than 50%.

[0004] Therefore, how to dispose of these solid wastes, or even how to utilize them in a high-value manner, is a technical problem that urgently needs to be solved. Summary of the Invention

[0005] To address the aforementioned problems, this invention aims to provide a high-performance microcrystalline glass based on multi-source solid waste and its preparation method.

[0006] The technical solution of the present invention is as follows:

[0007] On the one hand, a method for preparing high-performance glass-ceramics based on multi-source solid waste is provided, including the following steps:

[0008] S1: Obtain oil-based rock cuttings deoiling residue and phosphorus slag, and crush, dry, ball mill and sieve the oil-based rock cuttings deoiling residue and the phosphorus slag respectively to obtain residue powder and phosphorus slag powder.

[0009] S2: Perform component analysis on the phosphorus slag powder to confirm the MgO content in the phosphorus slag powder;

[0010] If the MgO content in the phosphorus slag powder is less than 15% of the total mass of the phosphorus slag powder, then the residue powder and the phosphorus slag powder are mixed, and after being mixed evenly, they are melted to obtain the basic glass melt.

[0011] If the MgO content in the phosphorus slag powder is less than 25% and greater than or equal to 15% of the total mass of the phosphorus slag powder, then the residue powder and the phosphorus slag powder are mixed with fly ash, and after being mixed evenly, they are melted to obtain the basic glass melt.

[0012] S3: The base glass liquid is quenched with water to obtain base glass, and the base glass is dried, ball-milled and sieved to obtain base glass powder;

[0013] S4: The base glass powder is placed in a mold and a sample preparation mechanism is used to obtain a microcrystalline glass sample. The microcrystalline glass sample is then sintered and naturally cooled to obtain the high-performance microcrystalline glass.

[0014] Preferably, in step S1, a sieve with a mesh size of 200 or larger is used for sieving.

[0015] Preferably, in step S2, when mixing, the amounts of each raw material by weight are 10-90 parts of residue powder, 10-50 parts of phosphorus slag powder, and 0-50 parts of fly ash.

[0016] Preferably, in step S2, during melting, the temperature is increased to 1350-1450°C at a rate of 5-7°C / min and held for 150-180min.

[0017] Preferably, in step S3, water quenching is performed using an immersion water quenching method.

[0018] Preferably, in step S3, when water quenching, the water is quenched in cold water at 10-20℃ for 5-10 minutes; when drying, the water is dried at 100-105℃ for 2-3 hours.

[0019] Preferably, in step S3, a sieve with a mesh size of 200 or larger is used for sieving.

[0020] Preferably, in step S4, when preparing the original microcrystalline glass sample, 0.5-1 mL of anhydrous ethanol or deionized water is added to the mold, and the sample is pressed for 10-15 s under a pressure of 8-10 MPa to obtain the original microcrystalline glass sample.

[0021] Preferably, in step S4, sintering is performed at 700-900℃ for 120-180 min.

[0022] On the other hand, a high-performance microcrystalline glass based on multi-source solid waste is also provided, which is prepared by the preparation method of high-performance microcrystalline glass based on multi-source solid waste as described in any one of the above.

[0023] The beneficial effects of this invention are:

[0024] (1) This invention utilizes oil-based rock debris deoiling residue as a raw material for sintering a high-performance microcrystalline glass, while assisting phosphorus slag in treating "waste" with "waste", realizing the synergistic high-value utilization of multi-source solid waste and solving the disposal problems of oil-based rock debris deoiling residue and phosphorus slag.

[0025] (2) The present invention can adjust the raw material ratio according to the different MgO content in the phosphorus slag to prepare CaO-Al2O3-SiO2 (CAS) microcrystalline glass and CaO-MgO-Al2O3-SiO2 (CMAS) microcrystalline glass.

[0026] (3) The present invention can successfully prepare CAS-based microcrystalline glass and CMAS-based microcrystalline glass without using any additional nucleating agent, and the properties of these microcrystalline glasses meet the requirements of the standard "Industrial Microcrystalline Sheets" (JC / T2097-2011) and are far higher than the lower limit of the requirements in the standard.

[0027] (4) The present invention uses phosphorus slag as raw material to provide MgO, which can prepare CAS-based microcrystalline glass and CMAS-based microcrystalline glass at a lower sintering temperature; and the prepared CMAS-based microcrystalline glass has better performance and lower sintering temperature than the microcrystalline glass prepared using pure MgO reagent.

[0028] (5) The preparation process of this invention is scientific and reasonable, the processing steps are simple and easy to implement, and the cost is relatively low; it can achieve large-scale production and generate economic benefits. Attached Figure Description

[0029] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments or the description of the present technology will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort or labor.

[0030] Figure 1 This is a schematic flowchart illustrating the preparation method of high-performance microcrystalline glass based on multi-source solid waste according to the present invention. Detailed Implementation

[0031] The present invention will be further described below with reference to the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and technical features described in this application can be combined with each other. It should also be pointed out that, unless otherwise indicated, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. The terms "comprising" or "including" and similar words used in this invention refer to elements or objects preceding the word that encompass the elements or objects listed following the word and their equivalents, without excluding other elements or objects.

[0032] On the one hand, such as Figure 1 As shown, this invention provides a method for preparing high-performance microcrystalline glass based on multi-source solid waste, comprising the following steps:

[0033] S1: Obtain oil-based rock cuttings deoiling residue and phosphorus slag, and crush, dry, ball mill and sieve the oil-based rock cuttings deoiling residue and the phosphorus slag respectively to obtain residue powder and phosphorus slag powder.

[0034] In one specific embodiment, a sieve with a mesh size of 200 or greater is used for sieving. It should be noted that the sieve mesh size in this embodiment is only a preferred sieve mesh size of the present invention. The higher the sieve mesh size, the finer the powder obtained. The fineness of different raw materials will affect the contact area between particles, which in turn will affect the diffusion of particles during sintering, ultimately leading to differences in the compactness of the microcrystalline glass structure. The finer the powder, the more beneficial it is to the performance of the microcrystalline glass.

[0035] S2: Perform component analysis on the phosphorus slag powder to confirm the MgO content in the phosphorus slag powder;

[0036] If the MgO content in the phosphorus slag powder is less than 15% of the total mass of the phosphorus slag powder, then the residue powder and the phosphorus slag powder are mixed, and after being mixed evenly, they are melted to obtain the basic glass melt.

[0037] If the MgO content in the phosphorus slag powder is less than 25% and greater than or equal to 15% of the total mass of the phosphorus slag powder, then the residue powder and the phosphorus slag powder are mixed with fly ash, and after being mixed evenly, they are melted to obtain the basic glass melt.

[0038] It should be noted that the method for determining the MgO content in phosphorus slag powder by component analysis is existing technology, and the specific analysis method will not be described in detail here.

[0039] In one specific embodiment, when mixing, the amounts of each raw material, by weight, are 10-90 parts of residue powder, 10-50 parts of phosphorus slag powder, and 0-50 parts of fly ash.

[0040] In the above embodiments, when the amount of fly ash is 0 parts, that is, the basic glass melt contains only residue powder and phosphorus slag powder, the microcrystalline glass obtained in the subsequent preparation is CAS-based microcrystalline glass; when the amount of fly ash is not 0 parts, that is, the basic glass melt contains not only residue powder and phosphorus slag powder but also fly ash, the microcrystalline glass obtained in the subsequent preparation is CMAS-based microcrystalline glass.

[0041] In one specific embodiment, during melting, the temperature is increased to 1350-1450°C at a rate of 5-7°C / min and held for 150-180min. It should be noted that there is no difference in the performance of the sample obtained by slowly heating to the target temperature and by directly placing the mixture at the target temperature; it is just that slowly heating the sample to the target temperature is more convenient and easier to melt.

[0042] S3: The base glass liquid is quenched with water to obtain base glass, and the base glass is dried, ball-milled and sieved to obtain base glass powder.

[0043] In one specific embodiment, immersion water quenching is used for water quenching. In this embodiment, immersion water quenching is used because it is simple and easy to implement, and the rapid cooling temperature of immersion water quenching can give the base glass a more uniform microstructure and stronger physical properties.

[0044] In one specific embodiment, water quenching is performed in cold water at 10-20°C for 5-10 minutes; drying is performed at 100-105°C for 2-3 hours.

[0045] In one specific embodiment, sieving is performed using a sieve with a mesh size of 200 or larger. In another specific embodiment, the base glass powder obtained by ball milling and passing it through sieves with different aperture sizes, wherein the aperture size ranges from 0.075 to 0.25 mm, is obtained.

[0046] It should be noted that the sieve mesh number in the above embodiments is only the preferred sieve mesh number of the present invention. The higher the sieve mesh number, the finer the powder obtained. The fineness of different raw materials will affect the contact area between particles, which in turn will affect the diffusion of particles during sintering, ultimately leading to differences in the compactness of the microcrystalline glass structure. The finer the powder, the more beneficial it is to the performance of microcrystalline glass.

[0047] S4: The base glass powder is placed in a mold and a sample preparation mechanism is used to obtain a microcrystalline glass sample. The microcrystalline glass sample is then sintered and naturally cooled to obtain the high-performance microcrystalline glass.

[0048] In one specific embodiment, when preparing the original microcrystalline glass sample, 0.5-1 mL of anhydrous ethanol or deionized water is added to the mold, and the sample is pressed for 10-15 s under a pressure of 8-10 MPa to obtain the original microcrystalline glass sample.

[0049] In the above embodiments, adding anhydrous ethanol or deionized water to the mold can wet the base glass powder so that it can be pressed and molded better.

[0050] In one specific embodiment, sintering is performed at 700-900°C for 120-180 minutes. Optionally, when the aforementioned base glass melt only includes residual powder and phosphorus slag powder, sintering is performed at 700-900°C for 120-180 minutes; when the aforementioned base glass melt includes not only residual powder and phosphorus slag powder but also fly ash, sintering is performed at 780-890°C for 120-180 minutes.

[0051] In this invention, CaO-Al2O3-SiO2 (CAS) or CaO-MgO-Al2O3-SiO2 (CMAS) microcrystalline glass can be prepared using the main components SiO2, Al2O3, and CaO in oil-based rock cuttings degreasing residue and the main components CaO, SiO2, Al2O3, and MgO (2%–25%) in phosphorus slag. During the preparation process, CaO acts as a flux, serving as an extracellular oxide in the glass body, providing a large amount of free oxygen to break Si-O-Si bonds, lowering the melting temperature of the glass, and reducing energy consumption. Al2O3 acts as an intermediate oxide in the glass body, increasing the degree of polymerization in the glass structure. SiO2, as the main component for glass formation, provides [SiO4] tetrahedra that form a large number of irregular network structures within the glass body, thus forming a glass skeleton, which can effectively improve the various properties of the microcrystalline glass. Furthermore, MgO in the phosphorus slag can act as a glass network modifier, enhancing the physical strength of the glass. Meanwhile, the oil-based rock cuttings deoiling residue and phosphorus slag also contain impurities such as Fe2O3, K2O, and P2O5, which can act as nucleating agents for microcrystalline glass, promoting its nucleation and crystallization. Based on the different MgO contents in the phosphorus slag's chemical composition, by adjusting the ratio of phosphorus slag to oil-based rock cuttings deoiling residue, CAS-based and CMAS-based microcrystalline glass can be prepared synergistically using both. When preparing CMAS-based microcrystalline glass, the relatively high MgO content in phosphorus slag leads to a decrease in the content of SiO2 and Al2O3. This invention uses fly ash to supplement SiO2 and Al2O3.

[0052] On the other hand, a high-performance microcrystalline glass based on multi-source solid waste is also provided, which is prepared by the preparation method of high-performance microcrystalline glass based on multi-source solid waste as described in any one of the above.

[0053] Example 1

[0054] A high-performance glass-ceramic based on multi-source solid waste is prepared through the following steps:

[0055] (1) Obtain oil-based rock cuttings deoiling residue and phosphorus slag, and crush, dry, ball mill and sieve the oil-based rock cuttings deoiling residue and the phosphorus slag respectively to obtain residue powder and phosphorus slag powder.

[0056] (2) The composition of the phosphorus slag powder is analyzed to confirm the content of MgO in the phosphorus slag powder and to prepare the basic glass melt;

[0057] In this embodiment, the MgO content in the phosphorus slag powder is less than 15% of the total mass of the phosphorus slag powder. The residue powder and the phosphorus slag powder are mixed in a dry state at a mass ratio of 50:50. After being mixed evenly, the mixture is placed in a muffle furnace and heated to 1350°C at 5°C / min and held for 180 min to obtain the basic glass melt.

[0058] (3) The base glass liquid is immersed in water quenching to obtain base glass, and the base glass is dried, ball-milled and sieved to obtain base glass powder;

[0059] In this embodiment, the drying process involves drying at 105°C for 2 hours and then sieving through a 200-mesh sieve.

[0060] (4) The base glass powder is placed in a mold and a sample preparation mechanism is used to obtain a microcrystalline glass sample. The microcrystalline glass sample is sintered and naturally cooled to obtain the high-performance microcrystalline glass.

[0061] In this embodiment, 3g of basic glass powder and 0.5mL of anhydrous ethanol with a mass fraction of 15% were added to the mold of the sample preparation machine and pressed under a pressure of 8MPa for 10s to obtain the original microcrystalline glass sample. The original microcrystalline glass sample was then placed in a muffle furnace and heated to 890℃ at 5℃ / min and held for 180min. After cooling with the furnace, the high-performance microcrystalline glass (CAS series microcrystalline glass) was obtained.

[0062] Example 2

[0063] Unlike Example 1, in this example, the mass ratio of the residue powder and the phosphorus slag powder in step (2) is 60:40.

[0064] Example 3

[0065] Unlike Example 1, in this example, the mass ratio of the residue powder to the phosphorus slag powder in step (2) is 70:30.

[0066] Example 4

[0067] Unlike Example 1, in this example, the mass ratio of the residue powder to the phosphorus slag powder in step (2) is 80:20.

[0068] Example 5

[0069] Unlike Example 1, in this example, the mass ratio of the residue powder to the phosphorus slag powder in step (2) is 90:10.

[0070] Example 6

[0071] Unlike Example 1, in this example, the mass ratio of the residue powder and the phosphorus slag powder in step (2) is 60:40; in step (4), during sintering, the original microcrystalline glass is placed in a muffle furnace and heated to 700°C at 5°C / min and held for 90 min, then heated to 900°C at 5°C / min and held for 90 min, and then cooled with the furnace to obtain the high-performance microcrystalline glass (CAS series microcrystalline glass).

[0072] Example 7

[0073] A high-performance glass-ceramic based on multi-source solid waste is prepared through the following steps:

[0074] (1) Obtain oil-based rock cuttings deoiling residue and phosphorus slag, and crush, dry, ball mill and sieve the oil-based rock cuttings deoiling residue and the phosphorus slag respectively to obtain residue powder and phosphorus slag powder.

[0075] (2) The composition of the phosphorus slag powder is analyzed to confirm the content of MgO in the phosphorus slag powder and to prepare the basic glass melt;

[0076] In this embodiment, the MgO content in the phosphorus slag powder is between 15% and 25% of the total mass of the phosphorus slag powder. The residue powder and the phosphorus slag powder are mixed with fly ash in a dry state at a mass ratio of 40:10:50. After being mixed evenly, the mixture is placed in a muffle furnace and heated to 1450°C at 5°C / min and held for 180 min to obtain the basic glass melt.

[0077] (3) The base glass liquid is immersed in water quenching to obtain base glass, and the base glass is dried, ball-milled and sieved to obtain base glass powder;

[0078] In this embodiment, the drying process involves drying at 105°C for 2 hours and then sieving through a 200-mesh sieve.

[0079] (4) The base glass powder is placed in a mold and a sample preparation mechanism is used to obtain a microcrystalline glass sample. The microcrystalline glass sample is sintered and naturally cooled to obtain the high-performance microcrystalline glass.

[0080] In this embodiment, 3g of basic glass powder and 0.5mL of anhydrous ethanol with a mass fraction of 15% were added to the mold of the sample preparation machine and pressed for 10s under a pressure of 8MPa to obtain the original microcrystalline glass sample. The original microcrystalline glass sample was then placed in a muffle furnace and heated to 880℃ at 5℃ / min and held for 180min. After cooling with the furnace, the high-performance microcrystalline glass (CMAS-based microcrystalline glass) was obtained.

[0081] Example 8

[0082] Unlike Example 7, in this example, the mass ratio of the residue powder and the phosphorus slag powder to the fly ash in step (2) is 30:20:50.

[0083] Example 9

[0084] Unlike Example 7, in this example, the mass ratio of the residue powder and the phosphorus slag powder to the fly ash in step (2) is 20:30:50.

[0085] Example 10

[0086] Unlike Example 7, in this example, the mass ratio of the residue powder and the phosphorus slag powder to the fly ash in step (2) is 10:40:50.

[0087] Example 11

[0088] Unlike Example 7, in this example, the mass ratio of the residue powder and the phosphorus slag powder to the fly ash in step (2) is 20:30:50; in step (4), during sintering, the original microcrystalline glass is placed in a muffle furnace and heated to 780°C at 5°C / min and held for 90 min, then heated to 890°C at 5°C / min and held for 90 min, and then cooled with the furnace to obtain the high-performance microcrystalline glass (CMAS-based microcrystalline glass).

[0089] Example 12

[0090] Unlike Example 11, in this example, step (3) of water quenching is not performed by immersion water quenching, but by pouring the base glass liquid into water for rapid cooling water quenching.

[0091] Comparative Example 1

[0092] Unlike Example 2, this comparative example uses a 60-mesh sieve for sieving in step (3).

[0093] Comparative Example 2

[0094] Unlike Example 2, this comparative example uses a 100-mesh sieve for sieving in step (3).

[0095] Comparative Example 3

[0096] A microcrystalline glass is prepared by the following steps:

[0097] (1) Obtain oil-based rock cuttings deoiling residue, and crush, dry, ball mill and sieve the oil-based rock cuttings deoiling residue to obtain residue powder;

[0098] (2) Preparation of the base glass melt;

[0099] The residue powder was mixed with pure MgO reagent and fly ash in a mass ratio of 42.5:7.5:50 under dry conditions. After being mixed evenly, the mixture was placed in a muffle furnace and heated to 1500℃ at 5℃ / min and held for 180min to obtain the basic glass melt.

[0100] (3) The base glass liquid is poured into water for rapid cooling and quenching to obtain base glass, and the base glass is dried, ball-milled and sieved to obtain base glass powder;

[0101] In this comparative example, the drying process was carried out at 105°C for 2 hours; the material was then sieved through a 200-mesh screen.

[0102] (4) The base glass powder is placed in a mold and a sample preparation machine is used to obtain a microcrystalline glass sample. The microcrystalline glass sample is sintered and naturally cooled to obtain the microcrystalline glass.

[0103] In this embodiment, 3g of basic glass powder and 0.5mL of anhydrous ethanol with a mass fraction of 15% were added to the mold of the sample preparation machine and pressed for 10s under a pressure of 8MPa to obtain the original microcrystalline glass sample. The original microcrystalline glass sample was then placed in a muffle furnace and heated to 850℃ at 5℃ / min and held for 90min. Then it was heated to 1000℃ at 5℃ / min and held for 90min. After cooling with the furnace, the microcrystalline glass (CMAS-based microcrystalline glass) was obtained.

[0104] Comparative Example 4

[0105] Unlike Comparative Example 3, in step (2) of this comparative example, the mass ratio of the residue powder to pure MgO reagent and fly ash is 45.5:4.5:50; in step (4), during sintering, the original sample of the microcrystalline glass is placed in a muffle furnace and heated to 800°C at 5°C / min and held for 90 min, then heated to 950°C at 5°C / min and held for 90 min, and then cooled with the furnace to obtain the microcrystalline glass (CMAS-based microcrystalline glass).

[0106] The performance of the microcrystalline glass obtained in each of the above embodiments and comparative examples was tested, and the test results are shown in Table 1:

[0107] Table 1. Performance test results of microcrystalline glass in each embodiment and comparative example.

[0108]

[0109]

[0110] As can be seen from Table 1, the CAS-based and CMAS-based microcrystalline glasses obtained in the various embodiments of the present invention all have good performance and can meet the requirements of the standard "Industrial Microcrystalline Sheets" JC / T 2097-2011. Since the main crystalline phases of the CMAS-based microcrystalline glass prepared by the present invention are orthopyroxene and diopside, its hardness is greater than that of the main crystalline phase wollastonite of the CAS-based microcrystalline glass. Therefore, the CMAS-based microcrystalline glass has a higher flexural strength than the CAS-based microcrystalline glass. The melting temperature of the CAS-based microcrystalline glass is lower than that of the CMAS-based microcrystalline glass. In addition, comparing Examples 11 and 12, it can be seen that the microcrystalline glass prepared by immersion water quenching has a higher flexural strength and other superior properties than the microcrystalline glass prepared by rapid cooling water quenching.

[0111] Comparing Example 2 of the present invention with Comparative Examples 1 and 2, it can be seen that the basic glass powder obtained by sieving with 60-mesh and 100-mesh sieves is too coarse (particle size greater than 0.075 mm). The resulting microcrystalline glass has low density and acid and alkali corrosion resistance, and high water absorption rate, which cannot meet the requirements of the standard "Industrial Microcrystalline Sheets" JC / T 2097-2011.

[0112] Comparing Example 11 of the present invention with Comparative Example 3 (calculated based on a MgO content of 25% in the phosphorus slag powder of Example 11) and Comparative Example 4 (calculated based on a MgO content of 15% in the phosphorus slag powder of Example 11), it can be seen that the properties of the CMAS-based microcrystalline glass prepared using pure MgO reagent are all inferior to those of the CMAS-based microcrystalline glass prepared in Example 11 of the present invention, and the sintering temperature used in Example 11 of the present invention is lower.

[0113] In addition, the heavy metal concentration and related indicators in the microcrystalline glass leachate of the present invention are far lower than those of the "Integrated Wastewater Discharge Standard" (GB 8978-1996) and the "Identification Standard for Hazardous Waste: Leaching Toxicity Identification" (GB 5085.3-2007), and will not cause secondary pollution to the environment, thus realizing the synergistic harmless treatment and high-value utilization of multi-source solid waste.

[0114] In summary, this invention enables the synergistic preparation of high-performance microcrystalline glass that meets the requirements of the standard "Industrial Microcrystalline Sheets" (JC / T 2097-2011) without the addition of additional nucleating agents, using oil-based rock cuttings degreasing residue and phosphorus slag as two solid wastes. Compared with the prior art, this invention represents a significant advancement.

[0115] The above description is merely a representative embodiment of the present invention and is not intended to limit the present invention in any way. Any embodiment made by those skilled in the art without departing from the scope of the present invention and utilizing the disclosed technical content is an equivalent embodiment of the present invention. Any simple modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention are still within the scope of the present invention.

Claims

1. A method for preparing high-performance glass-ceramics based on multi-source solid waste, characterized in that, The method comprises the following steps: S1: obtaining oil-based drilling debris deoiled residue and phosphorous slag, and crushing, drying, ball milling and sieving the oil-based drilling debris deoiled residue and the phosphorous slag respectively to obtain residue powder and phosphorous slag powder; S2: detecting the composition of the phosphorous slag powder to confirm the content of MgO in the phosphorous slag powder; if the content of MgO in the phosphorous slag powder is less than 15% of the total mass of the phosphorous slag powder, the residue powder and the phosphorous slag powder are mixed, and the mixture is melted to obtain a base glass liquid; if the content of MgO in the phosphorous slag powder is less than 25% and greater than or equal to 15% of the total mass of the phosphorous slag powder, the residue powder, the phosphorous slag powder and fly ash are mixed, and the mixture is melted to obtain a base glass liquid; when mixing, the amounts of the raw materials are 10-90 parts of residue powder, 10-50 parts of phosphorous slag powder and 0-50 parts of fly ash by weight; S3: water quenching the base glass liquid to obtain a base glass, drying, ball milling and sieving the base glass with a sieve mesh of greater than or equal to 200 to obtain a base glass powder; S4: placing the base glass powder in a mold to prepare a glass-ceramic sample by a sample preparation machine, and sintering the glass-ceramic sample to obtain the high-performance glass-ceramic after natural cooling; when the base glass liquid only comprises the residue powder and the phosphorous slag powder, the high-performance glass-ceramic obtained after sintering at 700-900 ℃ for 120-180 min and natural cooling is CAS glass-ceramic, and the main crystal phase is wollastonite; when the base glass liquid comprises the residue powder, the phosphorous slag powder and fly ash, the high-performance glass-ceramic obtained after sintering at 780-890 ℃ for 120-180 min and natural cooling is CMAS glass-ceramic, and the main crystal phases are augite and diopside.

2. The method for preparing high-performance microcrystalline glass based on multi-source solid waste according to claim 1, characterized in that, In step S1, sieving is performed with a sieve mesh of greater than or equal to 200.

3. The method for preparing high-performance microcrystalline glass based on multi-source solid waste according to claim 1, characterized in that, In step S2, when melting, the temperature is raised to 1350-1450 ℃ at a rate of 5-7 ℃ / min and maintained for 150-180 min.

4. The method for preparing high-performance microcrystalline glass based on multi-source solid waste according to claim 1, characterized in that, In step S3, water quenching is performed by a submerged water quenching method.

5. The method for preparing high-performance microcrystalline glass based on multi-source solid waste according to claim 1, characterized in that, In step S3, when water quenching, water quenching is performed in cold water at 10-20 ℃ for 5-10 min; when drying, drying is performed at 100-105 ℃ for 2-3 h.

6. The method for preparing high-performance microcrystalline glass based on multi-source solid waste according to claim 1, characterized in that, In step S4, when preparing the glass-ceramic sample, 0.5-1 mL of anhydrous ethanol or deionized water is further added to the mold, and the glass-ceramic sample is prepared by pressing at a pressure of 8-10 MPa for 10-15 s.

7. A high performance glass-ceramic based on multi-source solid waste, characterized in that, The high-performance glass-ceramic is prepared by the method of any one of claims 1-6.

Citation Information

Patent Citations

  • Method for preparing glass ceramics

    CN105731808A

  • High-strength low-density ceramsite proppant and preparation method thereof

    CN117776681A