CN103072954A - Method for producing colourless sulphuric acid by utilizing calcium sulfate - Google Patents
Method for producing colourless sulphuric acid by utilizing calcium sulfate Download PDFInfo
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- CN103072954A CN103072954A CN2013100059392A CN201310005939A CN103072954A CN 103072954 A CN103072954 A CN 103072954A CN 2013100059392 A CN2013100059392 A CN 2013100059392A CN 201310005939 A CN201310005939 A CN 201310005939A CN 103072954 A CN103072954 A CN 103072954A
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- sulfuric acid
- sulphuric acid
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- mixed gas
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Abstract
The invention relates to a method for producing colourless sulphuric acid by utilizing calcium sulfate. The method comprises the following steps: 1, performing high-temperature calcination on calcium sulfate powder, leading sulfur dioxide and oxygen gas mixture generated by calcination decomposition into an oxidation chamber to convert sulfur dioxide into sulfur trioxide, leading the obtained sulfur trioxide gas mixture into an absorption tower, and utilizing sulphuric acid in the absorption tower to spray input sulfur trioxide gas mixture in a circulating way, so that after sulphuric acid absorbs the sulfur trioxide gas in the gas mixture, the concentration is increased, and the yellow sulphuric acid with the concentration of 50-70 wt% is obtained; 2, using the obtained sulphuric acid to spray input sulfur trioxide gas mixture in a circulating way until the concentration of sulphuric acid is not less than 80 wt%; 3, drying the concentrated sulphuric acid until the concentration of concentrated sulphuric acid is not less than 98 wt%; and 4, heating to 100-200 DEG C and standing for 2-10 min, and filtering to obtain the filter liquor, namely the colourless sulphuric acid. The colourless sulphuric acid produced by the invention has the advantages of low content of product impurities and good quality.
Description
Technical field
The present invention relates to a kind of method of producing sulfuric acid, especially relate to a kind of method of utilizing calcium sulfate to produce colourless sulfuric acid.
Background technology
The sulfuric acid manufacture method that China is traditional, as raw material take sulphur or sulfurous iron ore, finish through steps such as high-temperature calcinations, the defective of its existence is, because contain a large amount of impurity in sulphur or the sulfurous iron ore, thereby be easy to occur side reaction in the relieving haperacidity process, its by product is easily sneaked in the sulfur dioxide gas, the centre is absorbed in the absorption tower, finally causes the sulfuric acid goods to present distinct colors.Most typical is exactly that iron ion is easy to make the sulfuric acid flavescence, affects quality and the outward appearance of sulfuric acid.
Increasingly exhausted along with sulphur and ferro-sulphur ore, the price of sulphur and sulfurous iron ore raw material also rises steadily, and the gas washing in SA production cost improves gradually, and therefore, the sulfuric acid of seeking new raw material, new explained hereafter better quality is imperative.
Summary of the invention
Technical problem to be solved by this invention is to provide the low calcium sulfate that utilizes of a kind of product foreign matter content to produce the method for colourless sulfuric acid.
The technical scheme that the present invention solves its technical problem employing is: a kind of method of utilizing calcium sulfate to produce colourless sulfuric acid may further comprise the steps:
(1) with calcium sulphate powders (preferred 1400-1600 ℃) calcining 30-60min under 1000-2000 ℃ of high temperature, the sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen are passed into the oxidizing chamber that contains the Vanadium Pentoxide catalyzer, reacting 20-50min under oxygen atmosphere and 400-600 ℃ of high temperature, is sulphur trioxide with Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into the absorption tower, utilize the sulphur trioxide mixed gas of the sulfuric acid circulated sprinkling input of the concentration 〉=30wt% in the absorption tower, behind the sulfur trioxide gas in the sulfuric acid absorption mixed gas, concentration raises, get the sulfuric acid of concentration 50-70wt%, be yellow;
(2) the sulphur trioxide mixed gas of step (1) gained sulfuric acid circulated sprinkling being inputted is to sulfuric acid concentration 〉=80wt%;
(3) with step (2) the gained vitriol oil under 0.1-1MPa (preferred 0.15-0.5MPa) pressure by containing anhydrous CaCl
2Moisture eliminator, absorb the moisture that the vitriol oil contains, to the concentration 〉=98wt% of the vitriol oil;
(4) step (3) the gained vitriol oil is heated to 100-200 ℃ and leave standstill 2-10min, the reduced viscosity of the vitriol oil, wherein accompanied by precipitation generates, and filters, and gets filtrate, is colourless sulfuric acid.
Further, in the step (1), the whiteness of described calcium sulphate powders 〉=80 degree, purity 〉=98wt%.
Because the vitriol oil has certain viscosity, thereby passes through CaCl
2Have certain pressure drop during powder for drying, and 0.1-1MPa (preferred 0.15-0.5MPa) pressure is provided, can make it pass through smoothly moisture eliminator.
It is owing to the wherein effect of contained ferric ion that sulphuric acid soln is yellow, and when the dilute sulphuric acid that will prepare was converted into the vitriol oil, the water molecules in the system was fewer and feweri, Fe
2(SO
4)
3Meltage also fewer and feweri, finally be converted into the precipitation and be removed.Add hot concentrated sulfuric acid and can reduce its viscosity, be convenient to filter the precipitation of generation.
The present invention prepares first dilute sulphuric acid take calcium sulfate as raw material, adopts circulated sprinkling and CaCl again
2The concentrated sulfuric acid of producing of dry method reduces moisture content, reduces Fe
2(SO
4)
3Meltage and separate out, filter, get colourless sulfuric acid, Fe in the product
2(SO
4)
3Foreign matter content is less than 0.05wt%.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Present embodiment may further comprise the steps:
(1) be 85 degree with the 1kg whiteness, purity is that the calcium sulphate powders of 98.2wt% is calcined 30min under 1450 ℃ of high temperature; The sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen being passed into the oxidizing chamber that contains the Vanadium Pentoxide catalyzer, react 20 min under oxygen atmosphere and 490 ℃ of high temperature, is sulphur trioxide with Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into the absorption tower, utilize the sulphur trioxide mixed gas of the sulfuric acid circulated sprinkling input of the concentration 30wt% in the absorption tower, behind the sulfur trioxide gas in the sulfuric acid absorption mixed gas, concentration raises, get the sulfuric acid of concentration 59wt%, be yellow;
(2) with the sulphur trioxide mixed gas of step (1) gained sulfuric acid circulated sprinkling input, to sulfuric acid concentration be 82wt%;
(3) with step (2) the gained vitriol oil under the 0.2MPa pressure condition by containing anhydrous CaCl
2Moisture eliminator, absorb the moisture that the vitriol oil contains, reach 98wt% to the concentration of the vitriol oil;
(4) step (3) the gained vitriol oil is heated to 200 ℃ and leave standstill 5min, the reduced viscosity of the vitriol oil, wherein accompanied by precipitation generates, and filters, and gets filtrate, is colourless sulfuric acid.
Fe in the colourless sulfuric acid of present embodiment gained
2(SO4)
3The content of impurity is 0.049wt%.
Embodiment 2
Present embodiment may further comprise the steps:
(1) be 88 degree with the 1kg whiteness, purity is that the calcium sulphate powders of 98.8wt% is calcined 45min under 1500 ℃ of high temperature; The sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen being passed into the oxidizing chamber that contains the Vanadium Pentoxide catalyzer, react 30min under oxygen atmosphere and 510 ℃ of high temperature, is sulphur trioxide with Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into the absorption tower, utilize the sulphur trioxide mixed gas of the sulfuric acid circulated sprinkling input of the concentration 35wt% in the absorption tower, behind the sulfur trioxide gas in the sulfuric acid absorption mixed gas, concentration raises, get the sulfuric acid of concentration 64wt%, be yellow;
(2) with the sulphur trioxide mixed gas of step (1) gained sulfuric acid circulated sprinkling input, to sulfuric acid concentration be 88wt%;
(3) with step (2) the gained vitriol oil under the 0.25MPa pressure condition by containing anhydrous CaCl
2Moisture eliminator, absorb the moisture that the vitriol oil contains, reach 98.5wt% to the concentration of the vitriol oil;
(4) step (3) the gained vitriol oil is heated to 200 ℃ and leave standstill 10min, the reduced viscosity of the vitriol oil, wherein accompanied by precipitation generates, and filters, and gets filtrate, is colourless sulfuric acid.
Fe in the colourless sulfuric acid of present embodiment gained
2(SO4)
3The content of impurity is 0.047wt%.
Embodiment 3
Present embodiment may further comprise the steps:
(1) be 90 degree with the 1kg whiteness, purity is that the calcium sulphate powders of 99.2wt% is calcined 50min under 1600 ℃ of high temperature; The sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen being passed into the oxidizing chamber that contains the Vanadium Pentoxide catalyzer, react 35 min under oxygen atmosphere and 540 ℃ of high temperature, is sulphur trioxide with Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into the absorption tower, utilize the sulphur trioxide mixed gas of the sulfuric acid circulated sprinkling input of the concentration 40wt% in the absorption tower, behind the sulfur trioxide gas in the sulfuric acid absorption mixed gas, concentration raises, get the sulfuric acid of concentration 69wt%, be yellow;
(2) with the sulphur trioxide mixed gas of step (1) gained sulfuric acid circulated sprinkling input, to sulfuric acid concentration be 92wt%;
(3) with step (2) the gained vitriol oil under the 0.3MPa pressure condition by containing anhydrous CaCl
2Moisture eliminator, absorb the moisture that the vitriol oil contains, reach 98.8wt% to the concentration of the vitriol oil;
(4) step (3) the gained vitriol oil is heated to 200 ℃ and leave standstill 15min, the reduced viscosity of the vitriol oil, wherein accompanied by precipitation generates, and filters, and gets filtrate, is colourless sulfuric acid.
Fe in the colourless sulfuric acid of present embodiment gained
2(SO4)
3The content of impurity is 0.045wt%.
Claims (2)
1. a method of utilizing calcium sulfate to produce colourless sulfuric acid is characterized in that, may further comprise the steps:
(1) calcium sulphate powders is calcined 30-60min under 1000-2000 ℃ of high temperature, the sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen are passed into the oxidizing chamber that contains the Vanadium Pentoxide catalyzer, reacting 20-50min under oxygen atmosphere and 400-600 ℃ of high temperature, is sulphur trioxide with Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into the absorption tower, utilize the sulphur trioxide mixed gas of the sulfuric acid circulated sprinkling input of the concentration 〉=30wt% in the absorption tower, behind the sulfur trioxide gas in the sulfuric acid absorption mixed gas, concentration raises, get the sulfuric acid of concentration 50-70wt%, be yellow;
(2) the sulphur trioxide mixed gas of step (1) gained sulfuric acid circulated sprinkling being inputted is to sulfuric acid concentration 〉=80wt%;
(3) with step (2) the gained vitriol oil under 0.1-1MPa pressure by containing anhydrous CaCl
2Moisture eliminator, absorb the moisture that the vitriol oil contains, to the concentration 〉=98wt% of the vitriol oil;
(4) step (3) the gained vitriol oil is heated to 100-200 ℃ and leave standstill 2-10min, the reduced viscosity of the vitriol oil, wherein accompanied by precipitation generates, and filters, and gets filtrate, is colourless sulfuric acid.
2. the method for utilizing calcium sulfate to produce colourless sulfuric acid according to claim 1 is characterized in that, in the step (1), and the whiteness of described calcium sulphate powders 〉=80 degree, purity 〉=98wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310005939.2A CN103072954B (en) | 2013-01-08 | 2013-01-08 | A kind of method utilizing calcium sulfate to produce colourless sulfuric acid |
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| CN201310005939.2A CN103072954B (en) | 2013-01-08 | 2013-01-08 | A kind of method utilizing calcium sulfate to produce colourless sulfuric acid |
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| CN103072954B CN103072954B (en) | 2016-04-27 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724338A (en) * | 2005-06-16 | 2006-01-25 | 什邡市鸿升化工有限公司 | Process for producing industrial sulfuric acid using phosphorus gypsum as raw material |
| CN1986390A (en) * | 2006-12-26 | 2007-06-27 | 四川泸天化股份有限公司 | Process of purifying and recovering waste sulfuric acid containing organic impurity |
| CN202369391U (en) * | 2011-12-14 | 2012-08-08 | 浙江嘉化能源化工股份有限公司 | Industrialized production device for liquid sulfur trioxide |
-
2013
- 2013-01-08 CN CN201310005939.2A patent/CN103072954B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724338A (en) * | 2005-06-16 | 2006-01-25 | 什邡市鸿升化工有限公司 | Process for producing industrial sulfuric acid using phosphorus gypsum as raw material |
| CN1986390A (en) * | 2006-12-26 | 2007-06-27 | 四川泸天化股份有限公司 | Process of purifying and recovering waste sulfuric acid containing organic impurity |
| CN202369391U (en) * | 2011-12-14 | 2012-08-08 | 浙江嘉化能源化工股份有限公司 | Industrialized production device for liquid sulfur trioxide |
Non-Patent Citations (1)
| Title |
|---|
| 谭德睿 等: "《艺术铸造》", 31 October 1996, 上海交通大学出版社 * |
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