CN1110665A - Production of ferrous sulfate monohydrate with liquid-phase forced dewatering method - Google Patents
Production of ferrous sulfate monohydrate with liquid-phase forced dewatering method Download PDFInfo
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- CN1110665A CN1110665A CN 95101641 CN95101641A CN1110665A CN 1110665 A CN1110665 A CN 1110665A CN 95101641 CN95101641 CN 95101641 CN 95101641 A CN95101641 A CN 95101641A CN 1110665 A CN1110665 A CN 1110665A
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- CN
- China
- Prior art keywords
- iron
- ferrous sulfate
- sulfate monohydrate
- dehydration
- vitriol
- 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.)
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- XBDUTCVQJHJTQZ-UHFFFAOYSA-L iron(2+) sulfate monohydrate Chemical compound O.[Fe+2].[O-]S([O-])(=O)=O XBDUTCVQJHJTQZ-UHFFFAOYSA-L 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007791 liquid phase Substances 0.000 title claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 38
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052742 iron Inorganic materials 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 27
- 230000018044 dehydration Effects 0.000 claims description 14
- 238000006297 dehydration reaction Methods 0.000 claims description 14
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims 2
- 239000001117 sulphuric acid Substances 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 239000012024 dehydrating agents Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 241000234435 Lilium Species 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- GDPKWKCLDUOTMP-UHFFFAOYSA-B iron(3+);dihydroxide;pentasulfate Chemical compound [OH-].[OH-].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GDPKWKCLDUOTMP-UHFFFAOYSA-B 0.000 description 1
- 201000004792 malaria Diseases 0.000 description 1
- 229940029985 mineral supplement Drugs 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The process features that under a certain condition, FeSO4.7H2O is forced to dewater sulfuric acid solution as dewatering agent to generate FeSO4.H2O. If sulfuric acid and iron or iron-containing material are used to produce FeSO4.H2O, the sulfuric must be first used as liquid-phase dewatering agent of FeSO4.7H2O and then takes part in reaction on iron or iron-containing material to generate FeSO4.7H2O. Its advantages include low energy consumption, high productivity and high quality of product.
Description
The invention provides a kind of novel method of producing the inorganic salt ferrous sulfate monohydrate.
As everyone knows, ferrous sulfate has purposes extremely widely in all many-sides such as industry, agricultural, forestry, and only fodder industry just reaches ten thousand tons at the annual consumption of China, but also is increasing year by year; Also rather considerable on the agricultural as little fertile its pent-up demand amount of using.In the market the most commonly with the ferrous sulfate of seven crystal water, producing the most general method of iron vitriol and be with sulfuric acid and scrap iron is that the raw material direct reaction makes.We know that iron vitriol character is very unstable, very easily weathering in the exsiccant air, and in malaria very easily oxidized generation yellowish brown ferric subsulfate.Iron vitriol product is on the market gone out to finally transporting to the user when using by manufacturer production, all exists the phenomenon of deterioration by oxidation more or less.This has brought more masty problem not only for packing, transportation and preservation etc., and finally can have influence on result of use.With the fodder industry is example, and after the iron vitriol that exists the deterioration by oxidation problem was sneaked into feed as trace mineral supplement, it was exactly inevitable that its bioavailability reduces.It has been recognized that some defectives of iron vitriol, begin to note having the ferrous sulfate monohydrate of suitable improvement, particularly in fodder industry, caused people's interest than iron vitriol character.
The a small amount of ferrous sulfate monohydrate commodity that occur on the market all are to be made through the gas phase drying and dehydrating by iron vitriol by classical way, as the described method of CN87102022A now.There are some problems in this method.At first owing to be subjected to the restriction of iron vitriol fusing point, drying must progressively be carried out, and is consuming time very long, and secondly the removing of six crystal water in the iron vitriol relies on thermal evaporation fully, and it is very big to consume energy.The dehydration of gas phase spraying drying may make shorten time of drying, but from aspects such as energy consumption, facility investment and technological operations, the cost of product will increase severely.At last, because time of drying is long, produce high price iron unavoidably in the product, and the particle degree of drying differ cause crystal water number irregularity, iron-holder is on the low side and unstable, this also is that on the market ferrous sulfate monohydrate product all is one of beige or linen major reason at present.As everybody knows, the ferrous sulfate monohydrate of standard should be lily.
The present invention has provided the method that solves the problems referred to above that ferrous sulfate monohydrate products production and quality product in the market exist, owing to easily implement, thereby have the value of commercial exploitation.
According to method of the present invention, provide two kinds of technological processs of producing ferrous sulfate monohydrate at this.Fig. 1 produces ferrous sulfate monohydrate by iron vitriol, and Fig. 2 is by sulfuric acid and iron or iron-bearing material production ferrous sulfate monohydrate, can introduce the present invention in detail in view of the above.
In the present invention, the dehydrating agent that at first places reactor is 50～98%(weight) sulfuric acid solution, stir and to rise to after 70～110 ℃ when progressively heating up or when temperature down, be that 1:3.00～30.00 join ferrous sulfate heptahydrate in the reactor in the dehydrating agent solution gradually by the weight ratio of dehydrating agent and ferrous sulfate heptahydrate, finish and keep 70～110 ℃ of dewatering system temperature. Because sulfuric acid has very strong dehydrating function, and just beginning dehydration at 64.4 ℃, ferrous sulfate heptahydrate is converted into ferrous sulfate monohydrate, therefore the present invention institute to system under the condition in the ferrous sulfate heptahydrate dehydration become the ferrous sulfate monohydrate pressure and carry out, this process is very fast, keep good stirring under 70～110 ℃, in 0.5～1.5 hour, can finish. The highly acid of dewatering system and faster dewatering speed got rid of oxidation of divalent and become ferric possibility, also so that the degree height of particle dehydration is consistent, this just provides very necessary condition for producing lily ferrous sulfate monohydrate product in good stirring. After dehydration is finished, carry out liquid-solid phase and separate, separation can adopt the mode of filtration to carry out. So far, dehydrating agent is owing to obtain the moisture content that ferrous sulfate heptahydrate loses, and itself has obtained dilution, after isolating through or still can be used as dehydrating agent and return use without adjusting, but must guarantee that the dehydrating agent sulfuric acid concentration is 50～98% in the reactor. Isolated ferrous sulfate monohydrate product can descend dry 0.5～1.0 hour at 80～100 ℃ then with a little ethanol washing, obtained at last meticulous, the lily ferrous sulfate monohydrate product of particle.
Below as can be seen, the whole process dewatering system is just kept necessary temperature in a short period of time, and time of drying is not long yet, so total energy consumption is very little; Simultaneously since in the reactor unit volume liquid-phase dehydration to handle capacity very big and process cycle is very short, so throughput is high, this be gas phase drying and dehydrating method production ferrous sulfate monohydrate can't compare.
Above-mentioned explanation can be described as the detailed explanation to Fig. 1.Fig. 2 is the extension of Fig. 1, and it produces iron vitriol from sulfuric acid and iron charge reaction.At this moment, sulfuric acid must be at first uses as the liquid-phase dehydration agent of iron vitriol, and after dehydration was finished, the dewatering agent after the dilution was isolated and spent the reaction that generates iron vitriol with iron or iron-bearing material again.We know, the vitriol oil can not be directly and the iron reaction generate iron vitriol, therefore present factory will go behind its thin up and the iron reaction again, promptly have the technological process of a concentrated acid dilution all the time.The present invention is quite different, except the production of first batch of iron vitriol needs the diluting concentrated sulfuric acid operation, continuous production has just saved this process, because in the present invention, the dilution of concentrated acid is to realize by the dehydration that obtains iron vitriol, and the vitriolic function has obtained fully playing among visible the present invention.
According to method of the present invention, under the secure situation of raw materials quality, can produce and contain ferrous iron and be not less than 32.0% pure white ferrous sulfate monohydrate product.
Embodiment 1:
In 500 milliliters beaker, insert 50% sulfuric acid, 195 grams, start and stir and intensification, progressively add iron vitriol 700 grams, finish and be warming up to 85～90 ℃ of continuation stirrings 1.0 hours, filter then, a little washing with alcohol of ferrous sulfate monohydrate, take out 80～90 ℃ of dryings 0.5 hour, claim to such an extent that the meticulous ferrous sulfate monohydrate 375 of pure white particle restrains.Its iron-holder is more than 32.0% after measured.
Claims (3)
1, a kind of novel method of producing ferrous sulfate monohydrate, it is characterized in that: ferrous sulfate monohydrate generates by making iron vitriol forced dehydration in the dewatering agent sulphuric acid soln under certain condition, and if with sulfuric acid and iron or iron-bearing material production ferrous sulfate monohydrate, then sulfuric acid must be at first uses as the liquid-phase dehydration agent of iron vitriol, just generates the reaction of iron vitriol then with iron or iron-bearing material.
2, method according to claim 1 is characterized in that iron vitriol when liquid phase is forced to dewater, and the dewatering agent that is adopted is a sulphuric acid soln, and its sulfuric acid concentration is 50～98%(weight); The weight ratio of dewatering agent and iron vitriol is 1:3.00～30.00; Dehydration temperaturre is 70～110 ℃; Dewatering time is 0.5～1.5 hour; In the whole dehydration, dewatering system is fully stirred.
3, method according to claim 1, it is characterized in that dewatering agent is finished becomes after the effect of ferrous sulfate monohydrate iron vitriol dehydration, itself has obtained dilution dewatering agent, from dewatering system, isolate then, can continue to serve as to the dewatering agent of iron vitriol or be used for generating the reaction of iron vitriol with iron or iron-bearing material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95101641 CN1110665A (en) | 1995-02-24 | 1995-02-24 | Production of ferrous sulfate monohydrate with liquid-phase forced dewatering method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95101641 CN1110665A (en) | 1995-02-24 | 1995-02-24 | Production of ferrous sulfate monohydrate with liquid-phase forced dewatering method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1110665A true CN1110665A (en) | 1995-10-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95101641 Pending CN1110665A (en) | 1995-02-24 | 1995-02-24 | Production of ferrous sulfate monohydrate with liquid-phase forced dewatering method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993117A (en) * | 2010-11-08 | 2011-03-30 | 新疆大学 | Normal-temperature production method for ferrous sulfate monohydrate |
| CN102892711A (en) * | 2010-05-17 | 2013-01-23 | 钛白粉欧洲有限公司 | Process for the production of ferrous sulphate monohydrate |
| CN106904663A (en) * | 2017-03-14 | 2017-06-30 | 襄阳龙蟒钛业有限公司 | A kind of method of utilization sulfuric acid method titanium pigment by-product production ferrous sulfate monohydrate |
| CN107108262A (en) * | 2014-12-09 | 2017-08-29 | 克罗内斯国际公司 | Process for reprocessing iron sulfate heptahydrate |
| CN115415037A (en) * | 2022-09-13 | 2022-12-02 | 铜陵翔瑞环保新材料有限公司 | Grinding process of ferrous sulfate monohydrate |
-
1995
- 1995-02-24 CN CN 95101641 patent/CN1110665A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102892711A (en) * | 2010-05-17 | 2013-01-23 | 钛白粉欧洲有限公司 | Process for the production of ferrous sulphate monohydrate |
| CN101993117A (en) * | 2010-11-08 | 2011-03-30 | 新疆大学 | Normal-temperature production method for ferrous sulfate monohydrate |
| CN101993117B (en) * | 2010-11-08 | 2013-07-17 | 新疆大学 | Normal-temperature production method for ferrous sulfate monohydrate |
| CN107108262A (en) * | 2014-12-09 | 2017-08-29 | 克罗内斯国际公司 | Process for reprocessing iron sulfate heptahydrate |
| CN106904663A (en) * | 2017-03-14 | 2017-06-30 | 襄阳龙蟒钛业有限公司 | A kind of method of utilization sulfuric acid method titanium pigment by-product production ferrous sulfate monohydrate |
| CN115415037A (en) * | 2022-09-13 | 2022-12-02 | 铜陵翔瑞环保新材料有限公司 | Grinding process of ferrous sulfate monohydrate |
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