CN111592040B - Method for removing cadmium in antimony trioxide production - Google Patents
Method for removing cadmium in antimony trioxide production Download PDFInfo
- Publication number
- CN111592040B CN111592040B CN202010641854.3A CN202010641854A CN111592040B CN 111592040 B CN111592040 B CN 111592040B CN 202010641854 A CN202010641854 A CN 202010641854A CN 111592040 B CN111592040 B CN 111592040B
- Authority
- CN
- China
- Prior art keywords
- cadmium
- antimony
- lead
- antimony trioxide
- antimony alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for removing cadmium in antimony trioxide production, which relates to the technical field of antimony trioxide production, and comprises the steps of after arsenic removal is finished, raising the temperature of a reflecting furnace to 1000-1200 ℃, and then adding a cadmium removing agent, wherein the adding amount is 0.5-1.5% of the weight of lead-antimony alloy liquid in the reflecting furnace; the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide with the mass ratio of 15-20; blowing air into the reverberatory furnace for 4-8 h, collecting the generated high-cadmium oxygen powder, and then obtaining cadmium-removed lead-antimony alloy; according to the method for removing cadmium in antimony trioxide production, the lead-antimony alloy raw material is subjected to arsenic removal and cadmium removal treatment, so that the arsenic content and the cadmium content in the antimony trioxide finished product are reduced, the antimony trioxide quality is improved, and the requirements of high-end industries can be met.
Description
Technical Field
The invention relates to the technical field of antimony trioxide production, in particular to a method for removing cadmium in antimony trioxide production.
Background
Antimony trioxide is an inorganic compound, the natural product is named as antimony white, commonly called as antimony white, white crystalline powder, the melting point is 655 ℃, the boiling point is 1550 ℃, the antimony trioxide is dissolved in sodium hydroxide solution, hot tartaric acid solution, tartaric acid hydrogen salt solution and sodium sulfide solution, and the antimony trioxide is slightly soluble in 370 +/-37 mu g/L water, dilute nitric acid and dilute sulfuric acid. It is widely used in the industries of enamel, pigment, paint, plastics, glass, ceramics and fireproof fabrics. The main application at present is used as a flame retardant synergist of plastics, chemical fiber substances and the like.
The preparation method of the antimony trioxide comprises a dry method and a wet method, wherein the dry method comprises a metallic antimony method and an stibnite method; the wet process includes an acid leaching process and an antimony salt decomposition process. The production raw materials are divided into two types: the first is single primary stibnite and the second is complex stibnite associated with other metals. Single ores are mined for decades, and the reserves are lower and lower than those of complex ores. In recent years, the attention is paid increasingly, and the application value of complex ores which are mined in large quantities is seriously influenced due to the problem that the lead and the antimony are difficult to separate in the smelting process. At present, the method for producing antimony trioxide by oxidizing lead-antimony alloy is widely used. The lead-antimony alloy is accompanied by impurities of arsenic and cadmium, and in the subsequent production process, the arsenic and cadmium enter the product antimony trioxide, so that the quality and the use of the antimony trioxide are influenced. In the existing production process, arsenic is generally removed, and cadmium is not removed independently, for example, the invention patent with the application number of CN201610439905.8, published as 20161109 discloses a method for producing antimony white, crude lead is smelted to remove copper, antimony and reduction smelting, so that lead-antimony alloy solution is obtained; removing arsenic from the lead-antimony alloy solution, and oxidizing and blowing to obtain antimony white. Only arsenic is removed, and cadmium is not removed, so that the cadmium content of the finished antimony trioxide product is higher.
Disclosure of Invention
The invention aims to solve the problems and provide a method for removing cadmium in antimony trioxide production, so that the arsenic content and the cadmium content in an antimony trioxide finished product are reduced, and the quality of antimony trioxide is improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for removing cadmium in antimony trioxide production comprises the following steps:
s1, after arsenic removal is finished, the temperature of the reverberatory furnace is increased to 1000-1200 ℃, and a cadmium removal agent is added, wherein the addition amount is 0.5-1.5% of the weight of the lead-antimony alloy liquid in the reverberatory furnace.
The cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide with the mass ratio of 15-20.
S2, continuously heating to 1000-1200 ℃, blowing air into the reverberatory furnace for 4-8 h, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
Preferably, in step S1, the specific process of removing arsenic is as follows: putting the raw material of the lead-antimony alloy into a reflecting furnace, heating and melting the raw material of the lead-antimony alloy into lead-antimony alloy liquid, adding an arsenic removal agent for reaction, and separating scum from the lead-antimony alloy liquid after the reaction is finished.
Preferably, the arsenic removing agent is sodium hydroxide or sodium carbonate.
Preferably, in step S1, the cadmium removing agent is composed of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 18.
Preferably, in step S1, the cadmium removing agent is added in an amount of 1%.
Preferably, in the step S2, the produced high cadmium oxide powder is collected in a cloth bag chamber.
Preferably, in step S2, the cadmium-removed lead-antimony alloy is subjected to oxidation converting to obtain antimony trioxide.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. according to the method for removing cadmium in the antimony trioxide production, the lead-antimony alloy raw material is subjected to arsenic removal and cadmium removal treatment, so that the arsenic content and the cadmium content in the antimony trioxide finished product are reduced, the quality of the antimony trioxide is improved, and the requirements of high-end industries can be met.
2. The cadmium removing agent comprises calcium phosphate, sodium chloride and silicon dioxide, excessive calcium phosphate is added to perform a replacement reaction with antimony and lead and form vitreous body high-melting-point slag with the silicon dioxide, and the vitreous body high-melting-point slag covers the surface of a melt in a furnace to inhibit volatilization of antimony and lead metal elements; the sodium chloride is added to reduce the volatilization temperature of impurity metal elements such as cadmium, copper and the like, accelerate the precipitation of cadmium and accelerate the precipitation of cadmium, and the combination of the three components can improve the removal rate of cadmium and improve the quality of antimony trioxide.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for removing cadmium in antimony trioxide production comprises the following steps:
s1, after arsenic removal is finished, raising the temperature of a reverberatory furnace to 1100 ℃, and adding a cadmium removal agent, wherein the adding amount is 1% of the weight of lead-antimony alloy liquid in the reverberatory furnace;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 18;
s2, continuously heating to 1100 ℃, blowing air into the reverberatory furnace for 6 hours, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
And S3, carrying out oxidation blowing on the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
Example 2
A method for removing cadmium in antimony trioxide production comprises the following steps:
s1, after arsenic removal is finished, raising the temperature of a reverberatory furnace to 1150 ℃, and adding a cadmium removal agent, wherein the adding amount is 1.5% of the weight of lead-antimony alloy liquid in the reverberatory furnace;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 20;
s2, continuously heating to 1150 ℃, blowing air into the reverberatory furnace for 4 hours, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
And S3, oxidizing and blowing the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
Example 3
A method for removing cadmium in antimony trioxide production comprises the following steps:
s1, after arsenic removal is finished, raising the temperature of a reverberatory furnace to 1200 ℃, and adding a cadmium removal agent, wherein the adding amount is 0.5 percent of the weight of lead-antimony alloy liquid in the reverberatory furnace;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 15.5;
s2, continuously heating to 1200 ℃, blowing air into the reverberatory furnace for 8 hours, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
And S3, oxidizing and blowing the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
Example 4
A method for removing cadmium in antimony trioxide production comprises the following steps:
s1, after arsenic removal is finished, raising the temperature of a reverberatory furnace to 1000 ℃, and adding a cadmium removal agent, wherein the adding amount is 0.5 percent of the weight of lead-antimony alloy liquid in the reverberatory furnace;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 15;
s2, continuously heating to 1000 ℃, blowing air into the reverberatory furnace for 6 hours, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
And S3, carrying out oxidation blowing on the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
Example 5
A method for removing cadmium in antimony trioxide production comprises the following steps:
s1, putting a lead-antimony alloy raw material into a reflecting furnace, heating and melting the raw material into lead-antimony alloy liquid, adding an arsenic removal agent for reaction, and separating floating slag from the lead-antimony alloy liquid after the reaction is finished. The arsenic removing agent is sodium hydroxide.
S2, after arsenic removal is finished, raising the temperature of the reverberatory furnace to 1100 ℃, and adding a cadmium removal agent, wherein the adding amount is 1% of the weight of the lead-antimony alloy liquid in the reverberatory furnace;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide in a mass ratio of 18;
and S3, continuously heating to 1100 ℃, blowing air into the reverberatory furnace for 6 hours, and collecting the generated high-cadmium oxygen powder to obtain the cadmium-removed lead-antimony alloy.
S4, oxidizing and blowing the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
Experimental example:
the cadmium contents of the lead-antimony alloy raw materials and the cadmium-removed lead-antimony alloys obtained in examples 1 to 4 and comparative example were measured by a flame atomic absorption method and the cadmium removal rate was calculated, and the results are shown in Table 1.
Cadmium removal rate = (cadmium content in lead-antimony alloy raw material-cadmium content in cadmium-removed lead-antimony alloy)/cadmium content in lead-antimony alloy raw material.
TABLE 1 analysis of the results
As can be seen from the data of examples 1-5 and Table 1, the method of the present invention can effectively remove cadmium from the lead-antimony alloy, thereby ensuring that the antimony trioxide finished product meets the national standard and can meet the requirements of high-end industries.
The cadmium removing agent comprises calcium phosphate, sodium chloride and silicon dioxide, excessive calcium phosphate is added to perform a replacement reaction with antimony and lead and form vitreous high-melting-point slag with the silicon dioxide, and the vitreous high-melting-point slag covers the surface of a melt in a furnace to inhibit volatilization of antimony and lead metal elements; the sodium chloride is added to reduce the volatilization temperature of impurity metal elements such as cadmium, copper and the like, accelerate the precipitation of cadmium and accelerate the precipitation of cadmium, and the combination of the three can improve the removal rate of cadmium and improve the quality of antimony trioxide. If no cadmium removing agent is added, a large amount of antimony and lead can volatilize together with cadmium, so that the aim of removing cadmium can not be achieved, and the waste of raw materials is caused. If the sodium chloride is not added, the reaction temperature needs to be increased, energy waste is caused, and the removal rate is influenced, but the addition of too much sodium chloride can cause the standard exceeding of chloride ions in the product, so the addition amount needs to be strictly controlled.
The above description is directed to the details of the preferred and possible embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (3)
1. A method for removing cadmium in antimony trioxide production is characterized by comprising the following steps:
s1, putting a lead-antimony alloy raw material into a reflecting furnace, heating and melting the raw material into lead-antimony alloy liquid, adding an arsenic removal agent for reaction, and separating floating slag from the lead-antimony alloy liquid after the reaction is finished; after arsenic removal is finished, the temperature of the reflecting furnace is increased to 1000-1200 ℃, and a cadmium removing agent is added, wherein the adding amount is 0.5-1.5% of the weight of the lead-antimony alloy liquid in the reflecting furnace; the addition amount of the cadmium removing agent is 1 percent;
the cadmium removing agent consists of calcium phosphate, sodium chloride and silicon dioxide with the mass ratio of 15-20;
s2, continuously heating to 1000-1200 ℃, blowing air into the reverberatory furnace for 4-8 hours, collecting the generated high cadmium oxygen powder, and collecting the generated high cadmium oxygen powder in a cloth bag chamber; obtaining cadmium-removed lead-antimony alloy; and (3) oxidizing and converting the cadmium-removed lead-antimony alloy to obtain antimony trioxide.
2. The method for removing cadmium in antimony trioxide production according to claim 1, wherein the arsenic removing agent is sodium hydroxide or sodium carbonate.
3. The method for removing cadmium in the production of antimony trioxide according to claim 1, wherein in the step S1, the cadmium removing agent is composed of calcium phosphate, sodium chloride and silica in a mass ratio of 18.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010641854.3A CN111592040B (en) | 2020-07-06 | 2020-07-06 | Method for removing cadmium in antimony trioxide production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010641854.3A CN111592040B (en) | 2020-07-06 | 2020-07-06 | Method for removing cadmium in antimony trioxide production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111592040A CN111592040A (en) | 2020-08-28 |
| CN111592040B true CN111592040B (en) | 2023-03-28 |
Family
ID=72188148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010641854.3A Active CN111592040B (en) | 2020-07-06 | 2020-07-06 | Method for removing cadmium in antimony trioxide production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111592040B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737020B (en) * | 2021-09-10 | 2022-09-13 | 广西万仕智稀贵金属科技有限公司 | Method for deeply removing cadmium in crude antimony refining process |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042653C (en) * | 1994-08-19 | 1999-03-24 | 锡矿山矿务局 | Stibium fire refining deleading agent, its preparation and application |
| CN104073659B (en) * | 2014-07-11 | 2016-02-17 | 湖南娄底华星锑业有限公司 | The method of lead, cadmium, iron is removed in a kind of coarse antimony refining |
| CN106086475A (en) * | 2016-06-17 | 2016-11-09 | 郴州市金贵银业股份有限公司 | The method producing stibium trioxide |
| CN111041233A (en) * | 2019-12-06 | 2020-04-21 | 广西万仕智稀贵金属科技有限公司 | Cadmium removing agent for antimony smelting production and application thereof |
-
2020
- 2020-07-06 CN CN202010641854.3A patent/CN111592040B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111592040A (en) | 2020-08-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101565174B (en) | Method for extracting refined tellurium from tellurium-contained smelting slag | |
| CA2798302C (en) | Process for recovering valuable metals from precious metal smelting slag | |
| CN102491287B (en) | Process for separating and recovering selenium from selenium-containing material | |
| CN106011488B (en) | A kind of method of high arsenic-and copper-bearing cigarette ash comprehensively recovering valuable metal | |
| CN107827089B (en) | Method for separating and recovering tellurium dioxide in cuprous telluride compound waste | |
| CN105154683A (en) | Method for separating and recycling valuable metal in tungsten slag | |
| CN101648702A (en) | Method for preparing tellurium dioxide by using crude tellurium as raw material | |
| CN103374658A (en) | Ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and method thereof | |
| CN106834707A (en) | A kind of method of arsenic-containing material synthetical recovery and arsenic recycling | |
| CN112609081A (en) | Method for producing electrolytic zinc by using high thallium zinc oxide | |
| CN111592040B (en) | Method for removing cadmium in antimony trioxide production | |
| CN109368688A (en) | A kind of production technology of high pure zinc oxide indirect method | |
| CN101525696B (en) | Method for leaching indium from leaching residue containing indium | |
| CN106884093A (en) | A kind of thick aurin smelting method | |
| CN109971945A (en) | A kind for the treatment of process of coarse tin decoppered slag | |
| CN113337724B (en) | Method for synchronously separating and extracting rare-dispersion element tellurium and metal copper from cuprous telluride slag | |
| CN110629042A (en) | Method for leaching antimony oxide material by tartaric acid system and producing metallic antimony by electrodeposition | |
| CN1042653C (en) | Stibium fire refining deleading agent, its preparation and application | |
| CN108893621A (en) | A kind of method of pyro-refining lead bullion | |
| CN109055764A (en) | A kind of comprehensive recovering process of the low zinc material of high chlorine | |
| CN104878198A (en) | Preparation method for leaded electrolyte | |
| CN109796049B (en) | Method for preparing iron oxide red by using iron slag precipitated by zinc hydrometallurgy goethite method | |
| CN113023689A (en) | Wet-method selenium refining process using lead-zinc smelting acid sludge as raw material | |
| JP4574826B2 (en) | How to recover tellurium | |
| KR101486669B1 (en) | Production of metalic tin from waste materials of the contain tin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |