CN1006882B - Wet process for producing sodium pyroantimonate - Google Patents
Wet process for producing sodium pyroantimonateInfo
- Publication number
- CN1006882B CN1006882B CN 85102490 CN85102490A CN1006882B CN 1006882 B CN1006882 B CN 1006882B CN 85102490 CN85102490 CN 85102490 CN 85102490 A CN85102490 A CN 85102490A CN 1006882 B CN1006882 B CN 1006882B
- Authority
- CN
- China
- Prior art keywords
- sodium
- sodium pyroantimonate
- temperature
- pyroantimoniate
- pressure
- 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.)
- Expired
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- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a wet process for producing sodium pyroantimonate, which belongs to coloured wet metallurgy. The process is characterized in that Sb2O3, NaOH and H2O2 are added into a reaction kettle in proportion; the sodium pyroantimonate ((Na2H2Sb2O7.6H2O) is generated by agitating reaction under the conditions of the temperature of 25 to 150 DEG C and the pressure of 1 to 3 atm. A reaction formula is expressed by that 2NaOH plus Sb2O3 plus 2H2O2 plus 4H2O is equal to Na2H2Sb2O7.6H2O, and a solution is crystallized. Crystallization conditions comprise the temperature of 0 to 160 DEG C and the pressure of 1 to 3 atm. Crystals are filtered and washed to obtain the sodium pyroantimonate. The sodium pyroantimonate is used as a high-grade glass clarifying agent and a fire retardation auxiliary agent, and the present invention has obvious economic benefits.
Description
The invention belongs to wet method and produce the method for sodium pyroantimoniate.Usually produce sodium pyroantimoniate pyrogenic process and wet method two class technologies are arranged.Thermal process is to make raw material with antimonous oxide, in the yellow soda ash medium, make oxygenant with SODIUMNITRATE, fusing at high temperature, reaction generates the positive sodium antimonate of pentavalent, and the reusable heat water logging goes out, positive sodium antimonate generation hydration reaction generates sodium pyroantimoniate (Tin Mine Mining Affairs Bureau " sodium pyroantimoniate pilot-plant test report (firing method process) "), in the wet processing, a kind of method is to make raw material with antimonous oxide, makes solvent with hydrochloric acid.Nitric acid is oxygenant, and with the antimonous oxide dissolved oxygen, reaction generates antimony pentachloride, uses the sodium hydroxide solution neutralization solution then, is settled out sodium pyroantimoniate (beautiful Qi chemical plant, Wuxi " O type glass fining agent assay certificate, No. (84) 001, tin section mirror word "); Another kind method is to be raw material with the antimony concentrate, leaches with sodium hydroxide and sodium sulfide solution, produces thioantimonious acid soda solution, blasts oxygen or atmospheric oxidation then in this solution, produces sodium pyroantimoniate (US4096232).Above-mentioned technology has following weak point: 1. adopts nitric acid or SODIUMNITRATE to make oxygenant, produces carcinogenic oxynitride, need higher expense processing environment pollution problem, and poor product quality; 2. directly produce sodium pyroantimoniate from antimony concentrate, quality product is low, and whiteness is poor; 3. the wet processing of dissolving with hydrochloric acid antimonous oxide, nitric acid oxidation sodium hydroxide neutralization precipitation is that ANTIMONY TRIOXIDE SB 203 99.8 PCT is become the solubility antimonic salt, consume a large amount of soda acids, the production cost height.
The purpose of this invention is to provide a kind of wet processing of producing sodium pyroantimoniate, this technology can adopt industrial antimonous oxide, directly participate in reaction with molecular conformation, in process of production, do not produce objectionable impurities, the sodium pyroantimoniate cost of producing is low, quality good, can be used as the finings or the flame retardant of high glass and teletube glass bulb.
The present invention makes raw material with industrial antimonous oxide, and sodium hydroxide solution is made solvent, and hydrogen peroxide is an oxygenant, produces the wet processing of sodium pyroantimoniate, and reaction is carried out crystallization after finishing, then after filtration, wash, dry white products.Two main phase producing process are: 1. step of reaction, and ANTIMONY TRIOXIDE SB 203 99.8 PCT, sodium hydroxide solution, hydrogen peroxide are added in the reactor of belt stirrer and heat, reactant reacts by following formula.
Temperature of reaction is in 25～150 ℃ of scopes, and pressure is 1～3atm.When temperature is 25～120 ℃, when pressure is 1～2.5atm, best results.The excess coefficient of alkali can be controlled in 1～4 scope, and preferably 1～3.The coefficient of excess of hydrogen peroxide is 1～1.6, is preferably 1～1.3.Reaction times generally needs 0.5～4 hour, becomes with treatment capacity.2. crystallisation stage, after reaction finished, solution was in same still or put to stirred type crystallizer and carry out crystallization, and Tc can change in 0～160 ℃ of scope.Pressure is controlled different crystallization conditions in 1～3atm, can produce varigrained sodium pyroantimoniate, and after crystallization was intact, the sodium pyroantimoniate filter dehydration oven dry with generating got white sodium pyroantimoniate.
The sodium pyroantimoniate quality of the present invention's preparation is good, total antimony 48.5 ± 0.5%; Sodium oxide 12.5 ± 0.5%, other impurity ferric oxide, cupric oxide, chromium sesquioxide, Vanadium Pentoxide in FLAKES etc. are all less than 0.05%, and crystal formation belongs to tetragonal system, and product meets teletron and fire retardant industry requirement; Whole technological process does not produce objectionable impurities; Do not need to transfer antimonous oxide to ionic condition, solvent consumption is few.
Example 1: with 50 gram antimonous oxides (industrial stibium trioxide), 70 milliliter 20% sodium hydroxide solution, 30 milliliter 35% hydrogen peroxide places reactor to stir after 10 minutes, be warming up to 110 ℃ again, and under this temperature, keep crystallization 6 hours,, get white sodium pyroantimoniate gained sedimentation and filtration, washing, oven dry.
Example 2: with 200 gram antimonous oxides (antimony oxygen), 200 milliliter 25% sodium hydroxide solution, 200 milliliter 30% hydrogen peroxide places the reactor heated and stirred, 95 ℃ of temperature of reaction, after 15 minutes, temperature is reduced to 60 ℃, under this temperature, kept stirred crystallization 8 hours, with crystal filter, wash, dry white sodium pyroantimoniate.
Claims (2)
1, a kind of is to make raw material with antimonous oxide, produces the wet processing of sodium pyroantimoniate, it is characterized in that using sodium hydroxide solution to be solvent, coefficient of excess 1～4; Hydrogen peroxide is an oxygenant, and coefficient of excess 1～1.3 is under 25～150 ℃ of temperature and pressure 1～3atm condition, oxidizing reaction generates sodium pyroantimoniate, the reaction finish after, crystallization under 0～160 ℃ of temperature, pressure 1～3atm condition, more after filtration, wash, dry the white powder sodium pyroantimoniate.
2,, it is characterized in that using the concentration of hydrogen peroxide is 30～35% by the described wet processing of producing sodium pyroantimoniate of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85102490 CN1006882B (en) | 1985-04-01 | 1985-04-01 | Wet process for producing sodium pyroantimonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85102490 CN1006882B (en) | 1985-04-01 | 1985-04-01 | Wet process for producing sodium pyroantimonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85102490A CN85102490A (en) | 1987-01-17 |
| CN1006882B true CN1006882B (en) | 1990-02-21 |
Family
ID=4792552
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85102490 Expired CN1006882B (en) | 1985-04-01 | 1985-04-01 | Wet process for producing sodium pyroantimonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1006882B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747229B (en) * | 2012-07-31 | 2013-11-27 | 中南大学 | Method for separating and recycling valuable metals in powder rich in multiple metals of waste circuit board |
| CN103318959A (en) * | 2013-07-15 | 2013-09-25 | 郴州市金贵银业股份有限公司 | Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation |
| CN107523702B (en) * | 2017-08-23 | 2019-03-19 | 中南大学 | A kind of method that the pressure oxidation of sodium salt system prepares sodium pyroantimonate |
| CN110015688B (en) * | 2018-01-09 | 2021-09-14 | 益阳生力材料科技股份有限公司 | Preparation method for reducing particle size of sodium pyroantimonate |
| CN110155960A (en) * | 2019-06-04 | 2019-08-23 | 淮北师范大学 | A kind of convenient and efficient preparation NaSbS2Method |
| CN113371757B (en) * | 2021-07-09 | 2022-11-08 | 中南大学 | Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor |
| CN115896488A (en) * | 2022-12-29 | 2023-04-04 | 广东先导稀材股份有限公司 | Method for extracting gallium from gallium antimonide material |
-
1985
- 1985-04-01 CN CN 85102490 patent/CN1006882B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85102490A (en) | 1987-01-17 |
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