CN113896239A - Preparation method of novel antimony trioxide - Google Patents
Preparation method of novel antimony trioxide Download PDFInfo
- Publication number
- CN113896239A CN113896239A CN202111245749.9A CN202111245749A CN113896239A CN 113896239 A CN113896239 A CN 113896239A CN 202111245749 A CN202111245749 A CN 202111245749A CN 113896239 A CN113896239 A CN 113896239A
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- Prior art keywords
- antimony trioxide
- temperature
- constant temperature
- antimony
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- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 18
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- -1 enamel Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K13/00—Thermometers specially adapted for specific purposes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of novel antimony trioxide, which sequentially comprises the following steps: the method comprises an antimony ingot oxidation and volatilization stage, a gradient cooling stage and a collection stage. By increasing the gradient cooling, the finally obtained antimony trioxide has stable crystal form, stable particle size distribution, stable dispersity, stable whiteness and better application effect. The invention is provided with an online detection system, and can adjust the process online according to the detection result, so that the final product has good uniformity.
Description
Technical Field
The invention relates to the field of antimony trioxide, in particular to a preparation method of novel antimony trioxide.
Background
Antimony trioxide has multiple purposes, can be used for manufacturing glass, enamel, medicines, bonding cement, fillers, mordant, fireproof coating and the like, can also be used as a flame retardant to be widely used in the industries such as plastics, rubber, textile, chemical fiber, pigment, paint, electronics and the like, and can also be used as a catalyst and a production raw material in the chemical industries such as petrochemical industry, synthetic fiber and the like.
The antimony trioxide is mainly used as a flame retardant, and many researches find that the crystal form and the grain diameter uniformity of the antimony trioxide are very important for flame retardance, and the crystal form and the grain diameter of two antimony trioxide with the purity of 99 percent have a difference of at least 30 percent for flame retardance, so that the preparation of the antimony trioxide with good crystal form and good grain diameter uniformity is very important.
Patent application publication No. CN112678869A discloses that making spherical structure by spheroidizing antimony trioxide with a sand mill and then making spherical antimony trioxide as seed crystal has better uniformity of particle size, but the whole process is very complicated, and polishing antimony trioxide in the actual production process is not good.
Disclosure of Invention
In order to solve the above problems, the present invention provides a novel method for preparing antimony trioxide,
sequentially comprises the following steps: the method comprises an antimony ingot oxidation and volatilization stage, a gradient cooling stage and a collection stage.
As a further aspect of the preparation method of the novel antimony trioxide of the present invention, the antimony ingot oxidation volatilization stage comprises: and putting the antimony ingot into a reverberatory furnace, melting at high temperature, and introducing mixed gas of air and oxygen to oxidize and gasify the antimony ingot.
As a further aspect of the method for producing a novel antimony trioxide of the present invention, wherein the gradient cooling stage comprises: and (3) passing the gasified antimony ingots through a quenching section, a first constant temperature section and a second constant temperature section in sequence.
As a further scheme of the preparation method of the novel antimony trioxide, the collection stage is that a cyclone separator enters a material receiving bin for collection.
As a further proposal of the preparation method of the novel antimony trioxide, the temperature of the high-temperature melting is 1000-1200 ℃.
As a further aspect of the method for preparing a novel antimony trioxide of the present invention, the mixed gas of air and oxygen is air: the volume ratio of oxygen is 8-10: 1.
as a further scheme of the preparation method of the novel antimony trioxide, the temperature of the quenching section is 400-500 ℃, the temperature of the first constant temperature section is 280-330 ℃, and the temperature of the second constant temperature section is 200-250 ℃.
As a further proposal of the preparation method of the novel antimony trioxide, the first constant temperature section and the second constant temperature section have the length of 20-25 m.
According to the invention, the online detection system can be used for online detection of the ventilation volume and the temperatures of the first constant temperature section and the second constant temperature section, and the adjustment of process conditions is linked according to the detection result, so that a product with good uniformity is finally obtained.
As a further scheme of the preparation method of the novel antimony trioxide, the position of an online detection port of the online detection system is positioned between the first constant-temperature section and the second constant-temperature section.
Specifically, when the particle size is smaller, the ventilation volume can be reduced or the temperature setting of the first constant temperature section and the second constant temperature section can be reduced; when the particle size is too large, the ventilation amount can be adjusted to be large or the temperature setting of the first constant temperature section and the second constant temperature section can be improved.
Specifically, the method for keeping the first constant temperature section and the second constant temperature section at constant temperature comprises the following steps: the outside of the pipe is wrapped with an interlayer which is filled with heat conducting oil, the outermost side is covered with a heat preservation layer, and the interlayer is externally connected with a heat conducting oil furnace for circulating heat preservation.
The technical scheme provided by the invention has the beneficial effects that:
by using the first constant temperature section and the second constant temperature section, the finally obtained antimony trioxide has stable grain size crystal form, stable grain size distribution, stable dispersity, stable whiteness and better application effect. The invention can adjust the process in time through the online detection system, and ensures that products in multiple batches or products in different time periods are very stable.
Detailed Description
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer.
Example 1
Adding antimony ingots into a reverberatory furnace for high-temperature melting, wherein the melting temperature is 1100 ℃, and introducing mixed gas of air and oxygen into the reverberatory furnace, wherein the ratio of air: the proportion of oxygen is 9: 1.
the gasified antimony trioxide is obtained at the moment, the smoke-dust-shaped antimony trioxide is obtained through a quenching section with the temperature of about 500 ℃, then the smoke-dust-shaped antimony trioxide sequentially passes through a first constant-temperature section with the temperature of about 330 ℃ and a second constant-temperature section with the temperature of 250 ℃, and finally enters a receiving bin through a cyclone separator, wherein the temperature of the receiving bin is 180 ℃.
Example 2
Adding antimony ingots into a reverberatory furnace for high-temperature melting, wherein the melting temperature is 1100 ℃, and introducing mixed gas of air and oxygen into the reverberatory furnace, wherein the ratio of air: the proportion of oxygen is 9: 1.
the gasified antimony trioxide is obtained at the moment, the smoke-like antimony trioxide is obtained through a quenching section with the temperature of about 450 ℃, then the smoke-like antimony trioxide sequentially passes through a first constant-temperature section with the temperature of about 300 ℃ and a second constant-temperature section with the temperature of 230 ℃, and finally enters a receiving bin through a cyclone separator, wherein the temperature of the receiving bin is 180 ℃.
Example 3
Adding antimony ingots into a reverberatory furnace for high-temperature melting, wherein the melting temperature is 1100 ℃, and introducing mixed gas of air and oxygen into the reverberatory furnace, wherein the ratio of air: the proportion of oxygen is 9: 1.
obtaining the gasified antimony trioxide, passing through a quenching section with the temperature of about 400 ℃ to obtain smoke-dust-shaped antimony trioxide, passing through a first constant-temperature section with the temperature of about 180 ℃ and a second constant-temperature section with the temperature of 200 ℃ in sequence, and finally passing through a cyclone separator to enter a receiving bin with the temperature of 180 ℃.
Example 4
Adding antimony ingots into a reverberatory furnace for high-temperature melting, wherein the melting temperature is 1100 ℃, and introducing mixed gas of air and oxygen into the reverberatory furnace, wherein the ratio of air: the proportion of oxygen is 9: 1.
the gasified antimony trioxide is obtained at the moment, the smoke-like antimony trioxide is obtained through a quenching section with the temperature of about 500 ℃, then the smoke-like antimony trioxide sequentially passes through a first constant-temperature section with the temperature of about 280 ℃ and a second constant-temperature section with the temperature of 200 ℃, and finally enters a receiving bin through a cyclone separator, wherein the temperature of the receiving bin is 180 ℃.
In order to illustrate the technical effects of the present invention, the particle size distribution, cubic crystal form, and whiteness of each example were tested. The cubic crystal form and the whiteness test method refer to GB/T4062-2013.
| Particle size D90 | Median diameter | Whiteness degree | Cubic crystal form | |
| Example 1 | ＜0.45um | 0.42um | 98.57％ | 98.57％ |
| Example 2 | ＜0.38um | 0.34um | 98.23％ | 99.03％ |
| Example 3 | ＜0.24um | 0.21um | 98.90％ | 99.10％ |
| Example 4 | ＜0.32um | 0.29um | 99.11％ | 98.76％ |
As can be seen from the table above, the particle size distribution obtained by the invention is very uniform, and the whiteness and the cubic crystal form are higher.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of novel antimony trioxide is characterized by sequentially comprising the following steps: the method comprises an antimony ingot oxidation and volatilization stage, a gradient cooling stage and a collection stage.
2. The method for preparing novel antimony trioxide according to claim 1, wherein the antimony ingot oxidation volatilization stage comprises: and putting the antimony ingot into a reverberatory furnace, melting at high temperature, and introducing mixed gas of air and oxygen to oxidize and gasify the antimony ingot.
3. The method of claim 1, wherein the gradient cooling stage comprises: and (3) passing the gasified antimony ingots through a quenching section, a first constant temperature section and a second constant temperature section in sequence.
4. The method for preparing the novel antimony trioxide as claimed in claim 1, wherein the collection stage is collection after entering a receiving bin by using a cyclone separator.
5. The method as claimed in claim 2, wherein the melting temperature at high temperature is 1000-1200 ℃.
6. The method for preparing a novel antimony trioxide as claimed in claim 2, wherein the mixed gas of air and oxygen is air: the volume ratio of oxygen is 8-10: 1.
7. the method as claimed in claim 3, wherein the temperature of the quenching section is 400-500 ℃, the temperature of the first constant temperature section is 280-330 ℃, and the temperature of the second constant temperature section is 200-250 ℃.
8. The method as claimed in claim 3, wherein the first constant temperature section and the second constant temperature section have a length of 20 to 25 m.
9. The method for preparing novel antimony trioxide as claimed in claim 3, characterized in that an online detection port of an online detection system is arranged between the first constant temperature section and the second constant temperature section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111245749.9A CN113896239A (en) | 2021-10-26 | 2021-10-26 | Preparation method of novel antimony trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111245749.9A CN113896239A (en) | 2021-10-26 | 2021-10-26 | Preparation method of novel antimony trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113896239A true CN113896239A (en) | 2022-01-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111245749.9A Pending CN113896239A (en) | 2021-10-26 | 2021-10-26 | Preparation method of novel antimony trioxide |
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| Country | Link |
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| CN (1) | CN113896239A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560493A (en) * | 2022-03-11 | 2022-05-31 | 广东长信精密设备有限公司 | Metal oxide powder production system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1873061A (en) * | 2006-04-27 | 2006-12-06 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN102616846A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| CN103508490A (en) * | 2013-08-23 | 2014-01-15 | 湖南辰州矿业股份有限公司 | Multi-functional upper expanding device for producing antimony trioxide |
| CN108622933A (en) * | 2018-06-08 | 2018-10-09 | 广东宇星阻燃新材股份有限公司 | A kind of antimony oxide powder crystal system |
-
2021
- 2021-10-26 CN CN202111245749.9A patent/CN113896239A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1873061A (en) * | 2006-04-27 | 2006-12-06 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN102616846A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| CN103508490A (en) * | 2013-08-23 | 2014-01-15 | 湖南辰州矿业股份有限公司 | Multi-functional upper expanding device for producing antimony trioxide |
| CN108622933A (en) * | 2018-06-08 | 2018-10-09 | 广东宇星阻燃新材股份有限公司 | A kind of antimony oxide powder crystal system |
Non-Patent Citations (1)
| Title |
|---|
| 雷霆 等: "《现代有色金属冶金科学技术丛书 锑冶金》", 28 February 2009, 冶金工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560493A (en) * | 2022-03-11 | 2022-05-31 | 广东长信精密设备有限公司 | Metal oxide powder production system |
| CN114560493B (en) * | 2022-03-11 | 2024-02-02 | 广东长信精密设备有限公司 | Metal oxide powder production system |
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220107 |
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