CN1077177A - Wet process for preparing soduim antimonate - Google Patents
Wet process for preparing soduim antimonate Download PDFInfo
- Publication number
- CN1077177A CN1077177A CN 92106876 CN92106876A CN1077177A CN 1077177 A CN1077177 A CN 1077177A CN 92106876 CN92106876 CN 92106876 CN 92106876 A CN92106876 A CN 92106876A CN 1077177 A CN1077177 A CN 1077177A
- Authority
- CN
- China
- Prior art keywords
- antimonate
- soduim
- preparing
- wet process
- tartrate
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims abstract description 20
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229940095064 tartrate Drugs 0.000 claims abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 6
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 claims description 3
- 229910019446 NaSb Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 2
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 239000002253 acid Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000722270 Regulus Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000006025 fining agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- LIYKJALVRPGQTR-UHFFFAOYSA-M oxostibanylium;chloride Chemical compound [Cl-].[Sb+]=O LIYKJALVRPGQTR-UHFFFAOYSA-M 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229940001516 sodium nitrate Drugs 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- YPMOSINXXHVZIL-UHFFFAOYSA-N sulfanylideneantimony Chemical compound [Sb]=S YPMOSINXXHVZIL-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- C01G30/02—Antimonates; Antimonites
- C01G30/023—Antimonates; Antimonites of ammonium, alkali or alkaline-earth metals or magnesium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a kind of is raw material with the thick weisspiessglanz of high arsenic, is auxiliary material with sodium hydroxide, carries out catalysis and oxidizing reaction, thereby produces the novel process of sodium antimonate.This technology comprises add sodium hydroxide solution, thick weisspiessglanz, tartrate and hydrogen peroxide in reactor, through stirring, in the reaction after 3-5 hours down of 40-150 ℃ of normal pressure and temperature, filters, cleans, dry white sodium antimonate.Advantage applies of the present invention reduces significantly at the production cost of sodium antimonate, is swift in response, and product matter is pure.
Description
The invention belongs to the sodium antimonate production technique, it is to be raw material with the thick weisspiessglanz of high arsenic, is auxiliary material with sodium hydroxide NaOH, through catalysis and oxide treatment, produces sodium antimonate.
It is that raw material is made the technology of sodium antimonate and is the technology that raw material is made sodium antimonate with the stibium trioxide that the method for producing at present both at home and abroad sodium antimonate is generally with the antimony sulfide.The former is with HCl and chlorine leaching, through repeatedly getting antimony oxychloride after the hydrolysis, adds the alkali neutralization again and makes sodium antimonate.This method complex process, long flow path, equipment corrosion is serious, waste water treatment difficulty, production cost height, unstable product quality.The latter generally is divided into two kinds, and the technology that provides as the flat 1-278424 of Japanese Patent is, stibium trioxide is dissolved in caustic soda soln, after filtration, adds hydrogen peroxide oxidation again and generate sodium antimonate in filtrate.This method is because stibium trioxide solubleness in caustic soda is very low, thereby direct yield is very low, the production cost height.Another kind is that the production method of raw material production sodium antimonate is to adopt SODIUMNITRATE to make oxygenant to calcine the generation sodium antimonate with soda ash in High Temperature Furnaces Heating Apparatus with the stibium trioxide, this method produces carcinogenic nitrogen dioxide waste gas, equipment complexity, poor product quality, the waste gas pollution control and treatment difficulty, the cost height.
The present invention is intended to overcome the deficiency of aforesaid method, simplifies technology, reduces cost, and improves the output and the quality of sodium antimonate.
Technical solution of the present invention is as follows:
In reactor, add sodium hydroxide solution, stir on the limit, the limit adds thick weisspiessglanz, add winestone acid as catalyst and hydrogen peroxide as oxidant simultaneously, with temperature of reaction control within the specific limits, normal pressure reacted several hours down, and then row filters, clean, after the drying, do not need crystallisation stage, directly get the white products sodium antimonate.In this scheme, except adopting the winestone acid as catalyst, also can adopt tartrate or oxalic acid.Tartrate and tartrate can use separately, also can mix use.The add-on of described three acid is generally the 0.5-10% of thick weisspiessglanz weight.
The embodiment of the invention:
Embodiment
In 1000 milliliters of reactors, inject the sodium hydroxide solution of 300 milliliters of 25-48%, add 150 grams while stirring and contain Sb
2O
394.8% and the thick weisspiessglanz of arsenic 2.7%, adding 7.5 gram tartrate and 160 ml concns simultaneously is the hydrogen peroxide of 27.5-35%, and control reaction temperature react 3-5 hour after-filtration between 65-95 ℃, with the clear water washing, and must the white products sodium antimonate after the drying treatment.This product contains NaSb(OH) 699.12%, contain trivalent antimony 0.09%.
Reaction is undertaken by following formula:
The sodium antimonate that generates is water insoluble, after filtration, washing, the dry white products that gets, impurity arsenic reaction back generates water-soluble sodium arseniate, enters mother liquor, and mother liquid evaporation is got the crystallization sodium arseniate, can be used as glass fining agent.
The thick weisspiessglanz of high arsenic that the present invention adopts is the work in-process of antimony regulus, cost than the stibium trioxide that blows with star metal will be at half, can reduce the production cost of sodium antimonate significantly, but the use accelerated reaction of tartrate or winestone salt, trivalent antimony in the product is dropped to below 0.1%, product color is very white, reacts under normal pressure and can carry out, and need not crystallisation stage.
Claims (6)
1, a kind of wet process for preparing soduim antimonate, employing sodium hydroxide is reaction solution, it is characterized in that in 300 milliliter 30% sodium hydroxide solution, adding the 150 thick weisspiessglanzs of gram and 7.5 gram tartrate and 160 milliliters of hydrogen peroxide, follow stirring, under normal pressure, in 40-150 ℃ of reaction 3-5 hour, after filtration, after the cleaning, dry white sodium antimonate, its reaction formula is:
2,, it is characterized in that in 300 milliliter 30% sodium hydroxide solution adding thick weisspiessglanz and 160 ml concns and be 27.5% H according to the described wet process for preparing soduim antimonate of claim 1
2O
2, in 40-150 ℃ of down reaction 3-5 hour, after filtration, cleaning, dry grey sodium antimonate.
3,, it is characterized in that described thick weisspiessglanz contains 94.8% Sb according to claim 1 or 2 described wet process for preparing soduim antimonate
2O
3With 2.7% arsenic.
4, according to the described wet process for preparing soduim antimonate of claim 1, it is characterized in that removing and adopt tartrate, also can adopt tartrate or oxalic acid.
5,, it is characterized in that tartrate and tartrate can use separately, also can mix use according to claim 1 or 4 described wet process for preparing soduim antimonate.
6,, it is characterized in that the white sodium antimonate of being produced contains 99.12% NaSb(OE according to the described wet process for preparing soduim antimonate of claim 1) 6 and 0.09% trivalent antimony.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106876 CN1077177A (en) | 1992-04-06 | 1992-04-06 | Wet process for preparing soduim antimonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106876 CN1077177A (en) | 1992-04-06 | 1992-04-06 | Wet process for preparing soduim antimonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1077177A true CN1077177A (en) | 1993-10-13 |
Family
ID=4942505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92106876 Pending CN1077177A (en) | 1992-04-06 | 1992-04-06 | Wet process for preparing soduim antimonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1077177A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371253C (en) * | 2005-05-13 | 2008-02-27 | 河南科技大学 | Process for Producing Sodium Antimonate Using Refined Antimony White |
| CN106745245A (en) * | 2016-11-22 | 2017-05-31 | 星贝达（北京）化工材料有限公司 | A kind of preparation method of sodium pyroantimonate and sodium metaantimonate |
| CN110629042A (en) * | 2019-11-05 | 2019-12-31 | 湖南工业大学 | A kind of tartaric acid system leaching antimony oxide material and method for electrowinning metal antimony |
| CN113772726A (en) * | 2021-09-22 | 2021-12-10 | 长沙烨星锑业有限公司 | Preparation method for producing sodium antimonate by using ethylene glycol antimony distillation residues |
-
1992
- 1992-04-06 CN CN 92106876 patent/CN1077177A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371253C (en) * | 2005-05-13 | 2008-02-27 | 河南科技大学 | Process for Producing Sodium Antimonate Using Refined Antimony White |
| CN106745245A (en) * | 2016-11-22 | 2017-05-31 | 星贝达（北京）化工材料有限公司 | A kind of preparation method of sodium pyroantimonate and sodium metaantimonate |
| CN110629042A (en) * | 2019-11-05 | 2019-12-31 | 湖南工业大学 | A kind of tartaric acid system leaching antimony oxide material and method for electrowinning metal antimony |
| CN110629042B (en) * | 2019-11-05 | 2021-11-26 | 湖南工业大学 | Method for leaching antimony oxide material by tartaric acid system and producing metallic antimony by electrodeposition |
| CN113772726A (en) * | 2021-09-22 | 2021-12-10 | 长沙烨星锑业有限公司 | Preparation method for producing sodium antimonate by using ethylene glycol antimony distillation residues |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination |