CN87102022A

CN87102022A - The technology of preparation-aqueous ferrous sulfate

Info

Publication number: CN87102022A
Application number: CN87102022.XA
Authority: CN
Inventors: 唐国干
Original assignee: Individual
Current assignee: Individual
Priority date: 1987-05-06
Filing date: 1987-05-06
Publication date: 1988-11-23
Also published as: CN1013103B

Abstract

A kind ofly prepare high purity, be difficult for the technology of the ferrous sulfate monohydrate of oxidation, this technology system adopt the thick green vitriol of sulfurous iron ore oxidation gained in damp atmosphere or preparation titanium dioxide byproduct---green vitriol is made raw material, carry through cleaning, boiling, concentrate, operation such as crystallization, drying and making, this prepared is simple, cost is low, its products obtained therefrom is difficult for deterioration by oxidation in damp atmosphere, thereby enlarge its range of application, this product is applicable to the raw material of making fodder additives in the herding, all can use in aquatic products, agricultural, chemical industry, medical treatment, food service industry simultaneously.

Description

The present invention relates to a kind ofly prepare the purity height, be difficult for the ferrous sulfate monohydrate (Feso of oxidation ₄H ₂O) technology.

In chemical industry dictionary and national chemical reagent products catalogue, point out ferrous sulfate (Feso ₄7H ₂O), be commonly called as green whetstone, blue-greenish colour monoclinic crystal, proportion 1.899(14.8 ℃), 64 ℃ of fusing points, lose six molecular crystal water at 90 ℃, lose whole crystal water, weathering gradually in air at 300 ℃, and oxidation and be tawny, anhydride is a white powder, and proportion is 3.4, then becomes blue-greenish colour again with the water effect, water-soluble, be dissolved in ethanol hardly, reductive action is arranged, natural product has melanterite, can be by iron and dilute sulphuric acid effect and make, specification GB664-77, the ferrous sulfate that the domestic market produces is iron vitriol (Feso ₄7H ₂O), many because of containing crystal water, in dry air weathering, rapid deterioration by oxidation in damp atmosphere, thereby limited its application.Still there are not a little producers of the ferrous sulfate monohydrate of production at home, national standard and province's standard of not working out ferrous sulfate monohydrate yet.

Task of the present invention provides a kind of green vitriol that utilizes, and prepares the purity height, is difficult for the technology of the ferrous sulfate monohydrate of oxidation, and this prepared is simple, and cost is low, and its products obtained therefrom is difficult for deterioration by oxidation in damp atmosphere, thereby enlarges its range of application.

To achieve these goals, solution of the present invention is, utilize green vitriol through clean, Zhu carries, and concentrates, operation such as crystallization, drying and making, and it is characterized in that utilizing sulfurous iron ore (FeS ₂) product-green vitriol of paying of the thick green vitriol that makes through oxidation in damp atmosphere or preparation titanium dioxide makes raw material, after cleaning the surfactant suspension material, put into iron pan or enamel reaction still, the ion exchanged water that adds six times of amounts dissolves, and adding 10% steel cuttings, its steel cuttings is in advance at 10%Na ₂CO ₃Zhu boils in the solution, after oil removing is derusted, and clean with the tap water flushing, heat Zhu then and boil to pH value 4.5～5.5, filter, if heavy metal content is less than 0.002% in the green vitriol, do not need removal of impurities, when heavy metal content greater than 0.002% the time, for removing the heavy metal in the product, can in solution, feed hydrogen sulfide, make it generate insoluble vitriol and remove.The clean steel cuttings that in filtrate, still adds green vitriol amount 10%, to absorb residual sulfuric acid root in the filtrate, thereby stablize acidity, filtrate is concentrated into 1/3～1/4 of original volume, left standstill crystallisation by cooling 12～14 hours, Tc is advisable at 10～25 ℃, with crystallization with a small amount of 95% washing with alcohol, and dry surperficial moisture content with whizzer, in stainless steel drying plant or loft drier, carry out drying then, be heated to 30～40 ℃ earlier, remove partial crystallization water, be heated to 90～120 ℃ then and dewater, remove six molecular crystal water, after crushed, obtain high purity, be difficult for oxidation white or linen ferrous sulfate monohydrate crystalline powder, in time be encapsulated in lucifuge the bottle in or in the packaging vessel.

The present invention compared with prior art has following advantage:

1. this product is white or canescence crystalline powder, odorless, and content is 95～98%, is a kind of high purity, is difficult for the ferrous sulfate monohydrate of oxidation;

2. this technology prices of raw and semifnished materials are cheap, and cost is low, are to utilize sulfurous iron ore (FeS ₂) byproduct-green vitriol of oxidation makes in damp atmosphere thick green vitriol or preparation titanium dioxide is made raw material, and domestic most employing iron and dilute sulphuric acid prepare iron vitriol;

3. of many uses, in herding, be used for the anaemia of livestock and poultry and make the raw material of fodder additives, on aquatic products, add copper sulfate with this product, be used to prevent and treat the material gill disease of fish, on agricultural, weedicide be can make, water purification agent, gas scavenger on chemical industry, are used as, and be used to make ink, pigment, metal surface, sanitas, as hematinic, its contained iron is synthetic blood red dirty raw material in the body in medical treatment, can treat modal hypoferric anemia, on food, can be used as additive.

Technical process of the present invention is: and thick green vitriol cleans → and Zhu carries → concentrates → crystallization → drying → pulverizing → packing → finished product.

Embodiment one:

Get sulfurous iron ore (FeS ₂) 3 kilograms of the thick green vitriols that make, remove its surperficial suspended impurity with the tap water flushing after, be put in iron pan or the enamel reaction still, add ion exchanged water and dissolve for 18 kilograms, and add 0.3 kilogram of steel cuttings, its steel cuttings is in advance through 10%Na ₂CO ₃Solution Zhu boils, and it is clean with the tap water flushing, heating Zhu then boils and is evaporated to pH value 4.5～5.5 and filters, in case of necessity (when heavy metal content greater than 0.002%) for removing heavy metal in the product, can in solution, feed hydrogen sulfide, make it generate insoluble vitriol and remove, in filtrate, still add 0.3 kilogram of clean steel cuttings,, stablize acidity to absorb remaining sulfate radical, be concentrated into original volume 1/3～1/4, left standstill crystallisation by cooling 12～14 hours, room temperature is 20 ℃, with crystallization with a small amount of 95% washing with alcohol, and dry surperficial moisture content with whizzer, moisture eliminator is put in crystallization carried out drying, remove partial crystallization water at 40 ℃ earlier, be warming up to 90～100 ℃ then and dewater, make 0.75 kilogram of ferrous sulfate monohydrate white powder, after tested result: FeSO ₄Content is 85.54%, calculates FeSO ₄H ₂O content is 95.67% or FeSO ₄7H ₂O content is 156.44%: acidity: show blue, pH value is 3.0～4.0.Heavy metal content is 0.002%; Arsenic salt: the arsenic spot does not show.

Embodiment two:

Get 5 kilograms of preparation titanium dioxide byproduct-green vitriols, after removing surfactant suspension impurity with tap water flushing, put into iron pan or enamel reaction still, add 0.5 kilogram of 30 kilograms of ion exchanged waters and clean steel cuttings, its steel cuttings pretreatment process is identical with embodiment one, heating Zhu then boils to pH value 4.5～5.5 and filters, it is identical with embodiment one to remove in the product heavy metal method in case of necessity, in filtrate, still add 0.5 kilogram of clean steel cuttings, be concentrated into 1/3～1/4 of original volume, left standstill crystallisation by cooling 12～14 hours, room temperature is 15 ℃, and crystallization with a small amount of 95% washing with alcohol, and is dried surperficial moisture content with whizzer, put into loft drier and carry out drying, be heated to 40 ℃ earlier and remove partial crystallization water, be heated to 90～100 ℃ then and dewater, remove six molecular crystal water, make 2.2 kilograms of ferrous sulfate monohydrate white powders, after tested result: FeSO ₄Content is 86.66%, calculates FeSO ₄H ₂O content is 96.88%, or FeSO ₄7H ₂O content is 158.64%, and acidity shows blue, and pH value is 3.0～4.0, and heavy metal content is 0.002%, arsenic salt: the arsenic spot does not show.

The present invention is along with the material purity difference, and recovery rate is generally 25～50%.

Claims

1, a kind of technology for preparing ferrous sulfate monohydrate, be through washing, Zhu carry, concentrate, operation such as crystallization, drying and making, it is characterized in that utilizing the thick green vitriol of sulfurous iron ore oxidation gained in damp atmosphere or preparation titanium dioxide byproduct--green vitriol is made raw material, after cleaning surfactant suspension impurity, add an amount of ion exchanged water and a small amount of clean steel cuttings, carry out that Zhu boils, filtering and impurity removing, still adding a small amount of clean steel cuttings in filtrate concentrates, leave standstill crystallisation by cooling, after a small amount of 95% washing with alcohol, carry out drying and dehydrating.

2, technology according to claim 1 is characterized in that the green vitriol that will clean adds the ion exchanged water of six times of amounts and 10% clean steel cuttings.

3, technology according to claim 1 and 2 is characterized in that heavy metal content for removing the heavy metal in the product, can feed hydrogen sulfide greater than 0.002 o'clock in the green vitriol in solution.

4, technology according to claim 1 and 2, it is characterized in that crystals dried temperature divides two constant temperature stages: the fs is 30～40 ℃, and subordinate phase is 90～120 ℃.