Method for preparing lead smelting slag glass-ceramics based on the oxidation of silicon-rich silicon smelting slag and composition adjustment

Patent metadata

Field	Value
Publication number	US-11964902-B2
Application number	US-202318389556-A
Country	US
Kind code	B2
Filing date	Nov 14, 2023
Priority date	Jun 29, 2021
Publication date	Apr 23, 2024
Grant date	Apr 23, 2024

Abstract

The invention discloses a method for preparing lead smelting slag glass-ceramics based on the oxidation of silicon-rich silicon smelting slag and composition adjustment, and belongs to the technical field of resource utilization of smelting slag rich in monatomic silicon. The method comprises the steps: mixing the silicon slag rich in monatomic silicon with an oxidant, a fluxing agent and a clarifying agent according to a formula ratio, ball-milling and screening to obtain a tempering raw material with uniform size, and performing high-temperature oxidation melting on the tempering raw material to form an oxidation-state molten tempering material; and carrying out further mixed melting on the molten tempering material and hot lead slag, carrying out water quenching to obtain basic glass, and carrying out heat treatment system on the obtained basic glass to form the glass ceramics. According to the method, the smelting slag rich in monatomic silicon is subjected to oxidation tempering and mixed melting with the hot lead slag to prepare the basic glass, and the glass ceramics are obtained by regulating and controlling the heat treatment system of the basic glass. The method is simple in technological process, high in production efficiency and low in cost, achieves the collaborative high-value conversion target of the silicon-rich silicon slag and the lead slag, and is easy to industrially popularize and apply.

First claim

We claim:

1. A method for preparing lead smelting slag glass-ceramics based on the oxidation of silicon-rich silicon smelting slag and composition adjustment, characterized in that raw material includes 35-55% lead slag and 45-65% oxidation tempering raw material, and the sum of mass percentages of the lead slag and the oxidation tempering raw material is 100%;
the oxidizing tempering raw material includes silicon slag, oxidant, flux and clarifier; the lead slag includes SiO 2 , CaO, Fe 2 O 3 , Al 2 O 3 , ZnO and MgO; the silicon slag includes SiO 2 , CaO, Al 2 O 3 , Na 2 O, KO, MgO and ZnO;
in the silicon slag, the weight ratio between SiO 2 , CaO, Al 2 O 3 , Na 2 O, K 2 O, MgO and ZnO is 65-72:12-18:8-12:0.6-2:0.4-1:0.2-1:0.1-1; silicon element in the silicon slag exists in the form of elemental silicon, silicon carbide and calcium yellow feldspar, and a weight ratio of elemental silicon, silicon carbide and calcium yellow feldspar is 15-30:30-60:5-10;
a weight ratio of SiO 2 , CaO, Fe 2 O 3 , Al 2 O 3 , ZnO and MgO in the lead slag is 32-36:10-20:20-30:5-10:2-6:1-4.

2. The method for preparing lead smelting slag glass-ceramics based on the oxidation of silicon-rich silicon smelting slag and composition adjustment according to claim 1 , characterized in that the oxidation tempering raw material is a combination of silicon slag, oxidant, flux and clarifier, a mass ratio of silicon slag, oxidant, flux and clarifier is 35-55:1-5:4-7:1-3;
the oxidant includes manganese dioxide and sodium nitrate, with a mass ratio of manganese dioxide to sodium nitrate being 1-4:0.5-5; the flux includes albite and borax, with a mass ratio of albite to borax being 2-6:0.3-4; the clarifier includes cerium oxide and sodium sulfate, with a mass ratio of cerium oxide to sodium sulfate being 1-2:0.5-3.

3. The method for preparing lead smelting slag glass-ceramics based on the oxidation of silicon-rich silicon smelting slag and composition adjustment according to claim 1 , comprising the following steps:
(1) prepare the oxidation tempering material in advance; weigh silicon slag, oxidant, flux and clarifier according to the formula amount to form an oxidation tempering batch; the oxidation tempering batch is melted to form an oxidation tempering material melt;
(2) prepare lead slag glass-ceramics; mix the oxidation tempering material melt formed in step (1) with hot lead slag and clarify it to form a basic glass liquid; the basic glass liquid is quenched with water, crushed, after formation and crystallization, crystallized glass is formed; the melting temperature is 1450-1500° C. and kept for 2-3 hours to obtain the oxidation tempering material melt;
conditions for mixing the oxidation tempering material melt and the hot lead slag are: mixing at 1500-1550° C. for 1-2.5 hours to form a glass liquid with uniform composition; transfer or pour the high-temperature glass liquid into pre-prepared water below 25° C., and the glass liquid instantly turns into glass particles; filter the glass particles out of the water and dry them at 120-170° C.;
crush the water-quenched basic glass frit in a crusher for 25-40 minutes, and then pass it through a 200-mesh sieve to obtain basic glass powder;

put the above basic glass powder into the mold, hold it under a pressure of 15-25 MPa for 15-25s and obtain a shaping body;
put the formed green body into the crystallization furnace and heat it up to 500-750° C. at a heating rate of 5-15° C./min for preheating for 2-5 hours, and then heat it up to 950-1100° C. at a heating rate of 3-8° C./min; Carry out heat preservation and sintering for 2-3 hours; lower the temperature to 830-960° C. at a cooling rate of 5-10° C./min, keep it for 1-2 hours and then naturally cool to room temperature to obtain glass-ceramics product.

Assignees

• Univ Beijing Technology

Inventors

• Wu Yufeng
• Liu Xiaomin
• Pan Dean

Classifications

• C03C10/0063 Primary

  containing waste materials, e.g. slags · CPC title

• C03B1/00

  Preparing the batches (chemical compositions C03C) · CPC title

• C03B19/063

  by hot-pressing powders · CPC title

• C03B19/1045

  by bringing hot glass in contact with a liquid, e.g. shattering · CPC title

• C03C1/002 Primary

  Use of waste materials, e.g. slags · CPC title