CN103072954B - A kind of method utilizing calcium sulfate to produce colourless sulfuric acid - Google Patents
A kind of method utilizing calcium sulfate to produce colourless sulfuric acid Download PDFInfo
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- CN103072954B CN103072954B CN201310005939.2A CN201310005939A CN103072954B CN 103072954 B CN103072954 B CN 103072954B CN 201310005939 A CN201310005939 A CN 201310005939A CN 103072954 B CN103072954 B CN 103072954B
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- sulfuric acid
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Abstract
Utilize calcium sulfate to produce a method for colourless sulfuric acid, comprise the following steps: (1), by calcium sulphate powders high-temperature calcination, by the sulfurous gas of calcining and decomposing generation, the mixed gas of oxygen passes into oxidizing chamber, is sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilizes the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, and obtains the sulfuric acid of concentration 50-70wt%, in yellow; (2) by the sulphur trioxide mixed gas that gained sulfuric acid circulated sprinkling inputs, to sulfuric acid concentration >=80wt%; (3) drying is carried out to the gained vitriol oil, to the concentration >=98wt% of the vitriol oil; (4) be heated to 100-200 DEG C and leave standstill 2-10min, filtering, obtain filtrate, be colourless sulfuric acid.Utilize the present invention to produce sulfuric acid, product foreign matter content is low, and quality is good.
Description
Technical field
The present invention relates to a kind of method of producing sulfuric acid, especially relate to a kind of method utilizing calcium sulfate to produce colourless sulfuric acid.
Background technology
The sulfuric acid manufacture method that China is traditional, for raw material with sulphur or sulfurous iron ore, complete through steps such as high-temperature calcinations, its defect existed is, owing to containing a large amount of impurity in sulphur or sulfurous iron ore, be thus easy to side reaction occurs in acid manufacturing processes, its by product is easily mixed in sulfur dioxide gas, centre is absorbed in absorption tower, finally causes sulfuric acid goods to present distinct colors.Most typical is exactly that iron ion is easy to sulfuric acid is turned yellow, and 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 gas washing in SA production cost improves gradually, therefore, find new raw material, new explained hereafter better quality sulfuric acid imperative.
Summary of the invention
Technical problem to be solved by this invention is, the calcium sulfate that utilizes providing a kind of product foreign matter content low produces the method for colourless sulfuric acid.
The technical scheme that the present invention solves the employing of its technical problem is: a kind of method utilizing calcium sulfate to produce colourless sulfuric acid, comprises the following steps:
(1) by calcium sulphate powders, under 1000-2000 DEG C of high temperature, (preferred 1400-1600 DEG C) calcines 30-60min, sulfurous gas calcining and decomposing produced, the mixed gas of oxygen pass into the oxidizing chamber containing Vanadium Pentoxide catalyzer, under oxygen atmosphere and 400-600 DEG C of high temperature, react 20-50min, be sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilize the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling of the concentration >=30wt% in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, obtain the sulfuric acid of concentration 50-70wt%, in yellow;
(2) by the sulphur trioxide mixed gas that step (1) gained sulfuric acid circulated sprinkling inputs, to sulfuric acid concentration >=80wt%;
(3) step (2) the gained vitriol oil is passed through containing anhydrous CaCl under 0.1-1MPa (preferred 0.15-0.5MPa) pressure
2moisture eliminator, absorb in the vitriol oil moisture contained, to the concentration>=98wt% of the vitriol oil;
(4) step (3) the gained vitriol oil be heated to 100-200 DEG C and leave standstill 2-10min, the viscosity of the vitriol oil reduces, and wherein accompanied by precipitation generates, and filters, obtains filtrate, be colourless sulfuric acid.
Further, in step (1), whiteness >=80 degree of described calcium sulphate powders, purity >=98wt%.
Because the vitriol oil has certain viscosity, thus pass through CaCl
2have certain pressure drop during powder for drying, and 0.1-1MPa (preferred 0.15-0.5MPa) pressure is provided, it can be made to pass through moisture eliminator smoothly.
Sulphuric acid soln is the effect due to ferric ion contained by wherein in yellow, and when the dilute sulphuric acid of preparation is converted into the vitriol oil, the water molecules in system is fewer and feweri, Fe
2(SO
4)
3meltage also fewer and feweri, be finally converted into precipitation and be removed.Add hot concentrated sulfuric acid and can reduce its viscosity, be convenient to filter the precipitation produced.
The present invention is raw material with calcium sulfate, first prepares dilute sulphuric acid, then adopts circulated sprinkling and CaCl
2dry method concentrates the sulfuric acid of production, reduces moisture content, reduces Fe
2(SO
4)
3meltage and separate out, filter, obtain colourless sulfuric acid, Fe in product
2(SO
4)
3foreign matter content is less than 0.05wt%.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The present embodiment comprises the following steps:
(1) be 85 degree by 1kg whiteness, purity is that the calcium sulphate powders of 98.2wt% calcines 30min under 1450 DEG C of high temperature; Sulfurous gas calcining and decomposing produced, the mixed gas of oxygen pass into the oxidizing chamber containing Vanadium Pentoxide catalyzer, and under oxygen atmosphere and 490 DEG C of high temperature, react 20min, be sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilize the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling of the concentration 30wt% in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, obtain the sulfuric acid of concentration 59wt%, in yellow;
(2) by the sulphur trioxide mixed gas that step (1) gained sulfuric acid circulated sprinkling inputs, be 82wt% to sulfuric acid concentration;
(3) step (2) the gained vitriol oil is passed through containing anhydrous CaCl under 0.2MPa pressure condition
2moisture eliminator, absorb in the vitriol oil moisture contained, the concentration to the vitriol oil reaches 98wt%;
(4) step (3) the gained vitriol oil be heated to 200 DEG C and leave standstill 5min, the viscosity of the vitriol oil reduces, and wherein accompanied by precipitation generates, and filters, obtains filtrate, be colourless sulfuric acid.
Fe in the colourless sulfuric acid of the present embodiment gained
2(SO4)
3the content of impurity is 0.049wt%.
Embodiment 2
The present embodiment comprises the following steps:
(1) be 88 degree by 1kg whiteness, purity is that the calcium sulphate powders of 98.8wt% calcines 45min under 1500 DEG C of high temperature; Sulfurous gas calcining and decomposing produced, the mixed gas of oxygen pass into the oxidizing chamber containing Vanadium Pentoxide catalyzer, and under oxygen atmosphere and 510 DEG C of high temperature, react 30min, be sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilize the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling of the concentration 35wt% in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, obtain the sulfuric acid of concentration 64wt%, in yellow;
(2) by the sulphur trioxide mixed gas that step (1) gained sulfuric acid circulated sprinkling inputs, be 88wt% to sulfuric acid concentration;
(3) step (2) the gained vitriol oil is passed through containing anhydrous CaCl under 0.25MPa pressure condition
2moisture eliminator, absorb in the vitriol oil moisture contained, the concentration to the vitriol oil reaches 98.5wt%;
(4) step (3) the gained vitriol oil be heated to 200 DEG C and leave standstill 10min, the viscosity of the vitriol oil reduces, and wherein accompanied by precipitation generates, and filters, obtains filtrate, be colourless sulfuric acid.
Fe in the colourless sulfuric acid of the present embodiment gained
2(SO4)
3the content of impurity is 0.047wt%.
Embodiment 3
The present embodiment comprises the following steps:
(1) be 90 degree by 1kg whiteness, purity is that the calcium sulphate powders of 99.2wt% calcines 50min under 1600 DEG C of high temperature; Sulfurous gas calcining and decomposing produced, the mixed gas of oxygen pass into the oxidizing chamber containing Vanadium Pentoxide catalyzer, and under oxygen atmosphere and 540 DEG C of high temperature, react 35min, be sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilize the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling of the concentration 40wt% in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, obtain the sulfuric acid of concentration 69wt%, in yellow;
(2) by the sulphur trioxide mixed gas that step (1) gained sulfuric acid circulated sprinkling inputs, be 92wt% to sulfuric acid concentration;
(3) step (2) the gained vitriol oil is passed through containing anhydrous CaCl under 0.3MPa pressure condition
2moisture eliminator, absorb in the vitriol oil moisture contained, the concentration to the vitriol oil reaches 98.8wt%;
(4) step (3) the gained vitriol oil be heated to 200 DEG C and leave standstill 15min, the viscosity of the vitriol oil reduces, and wherein accompanied by precipitation generates, and filters, obtains filtrate, be colourless sulfuric acid.
Fe in the colourless sulfuric acid of the present embodiment gained
2(SO4)
3the content of impurity is 0.045wt%.
Claims (2)
1. utilize calcium sulfate to produce a method for colourless sulfuric acid, it is characterized in that, comprise the following steps:
(1) calcium sulphate powders is calcined 30-60min under 1000-2000 DEG C of high temperature, sulfurous gas calcining and decomposing produced, the mixed gas of oxygen pass into the oxidizing chamber containing Vanadium Pentoxide catalyzer, under oxygen atmosphere and 400-600 DEG C of high temperature, react 20-50min, be sulphur trioxide by Sulphur Dioxide; Gained sulphur trioxide mixed gas is passed into absorption tower, utilize the sulphur trioxide mixed gas that the sulfuric acid circulated sprinkling of the concentration >=30wt% in absorption tower inputs, after the sulfur trioxide gas in sulfuric acid absorption mixed gas, concentration raises, obtain the sulfuric acid of concentration 50-70wt%, in yellow;
(2) by the sulphur trioxide mixed gas that step (1) gained sulfuric acid circulated sprinkling inputs, to sulfuric acid concentration >=80wt%;
(3) step (2) the gained vitriol oil is passed through containing anhydrous CaCl under 0.1-1MPa pressure
2moisture eliminator, absorb in the vitriol oil moisture contained, to the concentration>=98wt% of the vitriol oil;
(4) step (3) the gained vitriol oil be heated to 100-200 DEG C and leave standstill 2-10min, the viscosity of the vitriol oil reduces, and wherein accompanied by precipitation generates, and filters, obtains filtrate, be colourless sulfuric acid.
2. the method utilizing calcium sulfate to produce colourless sulfuric acid according to claim 1, is characterized in that, in step (1), and whiteness >=80 degree of described calcium sulphate powders, 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 true 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 |
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