CN112499690A - Preparation method of crystal seed for treating brushing water - Google Patents
Preparation method of crystal seed for treating brushing water Download PDFInfo
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- CN112499690A CN112499690A CN202011502700.2A CN202011502700A CN112499690A CN 112499690 A CN112499690 A CN 112499690A CN 202011502700 A CN202011502700 A CN 202011502700A CN 112499690 A CN112499690 A CN 112499690A
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- 239000013078 crystal Substances 0.000 title claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 230000001680 brushing effect Effects 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 39
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 20
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 20
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 20
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 11
- 229910001448 ferrous ion Inorganic materials 0.000 claims abstract description 8
- 230000007547 defect Effects 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 230000001131 transforming effect Effects 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 15
- 238000005554 pickling Methods 0.000 abstract description 13
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 238000005201 scrubbing Methods 0.000 abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 7
- 239000010935 stainless steel Substances 0.000 abstract description 7
- BIJOYKCOMBZXAE-UHFFFAOYSA-N chromium iron nickel Chemical compound [Cr].[Fe].[Ni] BIJOYKCOMBZXAE-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 36
- 239000002253 acid Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000011651 chromium Substances 0.000 description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229960005191 ferric oxide Drugs 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 229910000604 Ferrochrome Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a preparation method of a crystal seed for treating brushing water, belonging to the field of recycling of industrial three wastes. The preparation method of the crystal seed for treating the brushing water comprises the steps of preparing or preparing a solution containing ferrous ions, adjusting the pH value of the solution, adding hydrogen peroxide for reaction, standing and aging and the like; the ferrous sulfate is preferably used for preparing the solution, the ferrous sulfate is used for preparing the ferroferric oxide crystal seeds by in-situ synthesis at normal temperature, the ferroferric oxide crystal seeds have the amorphous characteristic, the crystal lattices have defects and strong activity, the metal ions in the scrubbing water can be efficiently removed in the implementation and application, the nickel-chromium-iron crystal ore can be recovered, and the problem that the prior art cannot effectively recycle the stainless steel pickling scrubbing water can be effectively solved.
Description
Technical Field
The invention belongs to the field of recycling of industrial three wastes, relates to recycling of industrial waste liquid, and particularly relates to a preparation method of a crystal seed for treating brushing water.
Background
The aim of stainless steel pickling is mainly to remove iron scales and other surface defects generated in the heating and rolling processes, most of hot-rolled stainless steel pickling in China adopts sulfuric acid pickling and mixed acid pickling, a roller scrubbing and cleaning section is arranged between a sulfuric acid washing tank and a mixed acid washing tank and between the mixed acid washing tank and a steel coil collection in a pickling line, and the aim of removing deposits generated by pickling the surface of a steel plate out of the tank and washing away acid liquor brought out of the tank is achieved. The stainless steel pickling mainly generates two waste liquids, namely waste acid generated in a pickling section and scrubbing water generated in a cleaning section. The brushing water is one of waste liquid discharged in the stainless steel pickling process, has the characteristics of large water quantity and low contents of free acid and metal ions compared with concentrated waste acid discharged in the same way, and is weakly acidic waste water with light pollution degree.
At present, the method for treating the brushing water mainly comprises the steps of mixing waste acid with the brushing water, and then carrying out lime neutralization precipitation treatment, wherein a large amount of acid mud and filtered water are generated by neutralization precipitation, chromium is precipitated in the acid mud as trivalent hydroxide, the trivalent chromium hydroxide existing in a monomer of the chromium is oxidized into hexavalent chromium in the air, and the chromium becomes dangerous solid waste during stacking, so that great pollution is caused to the environment.
The content of free acid, metal ions and the like in the brushing water is low, but the discharge amount is large, so the brushing water is diluted acid water which is easy to treat. The brushing water is mixed into the waste acid with high content of free acid and metal ions, so that the brushing water can only be treated together according to the waste acid, thereby increasing the treatment capacity of the waste acid, increasing the treatment cost and having higher medicament cost; although a large amount of water can reach the standard discharge, the water resource is wasted. The brushing water and the concentrated waste acid are treated in a classified way, so that the brushing water is prevented from becoming waste acid liquid which is difficult to treat when the brushing water and the concentrated waste acid are mixed. The classified independent treatment of the brushing water with relatively clear pollution degree reduces the corresponding water treatment cost, and is beneficial to the targeted resource recovery of water and acid respectively.
Disclosure of Invention
The invention aims to solve the technical problem that the prior art cannot effectively utilize the stainless steel pickling and brushing water as resources.
The technical scheme adopted by the invention for solving the technical problem is to provide a crystal seed preparation method for treating the washing water, the crystal seed prepared by the method can effectively carry out resource utilization on the stainless steel acid washing water, and the method comprises the following steps:
a. preparing or preparing a solution containing ferrous ions;
b. adding a pH regulator into the solution obtained in the step a, and regulating the pH of the solution to be 8-9 stably;
c. b, adding a transforming agent into the solution obtained in the step b until the solution is changed from blue green to black;
d. and d, standing and aging the solution obtained in the step c to obtain a seed crystal liquid containing ferroferric oxide seed crystals.
In the step a, the solution containing the ferrous ions is prepared or prepared as a ferrous sulfate solution.
Further, the concentration of the ferrous sulfate solution is 20-25%.
In the step b, the pH regulator is at least one of sodium carbonate and sodium hydroxide.
Further, the pH regulator is a sodium hydroxide solution with a concentration of 25-35%.
In the step c, the converting agent is at least one of oxygen, air and hydrogen peroxide.
And c, performing the steps b and c under the stirring condition.
And d, filtering the seed crystal liquid obtained in the step d to obtain ferroferric oxide seed crystals.
The ferroferric oxide crystal seed prepared by the method is synthesized in situ by ferrous iron, and has amorphous shape, crystal defects and high reaction activity.
The invention has the beneficial effects that: magnetite which takes ferroferric oxide as a main component, and the ferroferric oxide iron sheet formed by steel rolling production cannot be used as seed crystal because the iron and chromium can not be induced to crystallize by taking the ferroferric oxide as a crystal nucleus in the brushing water because of complete crystallization and low activity. When ferrous sulfate is used for preparing ferroferric oxide conventionally, ferric oxide is used as a batch, the required reaction temperature is above 100 ℃, the reaction time is long, and the generated ferroferric oxide has the advantages of complete crystallization, compact structure, larger particles, low activity and unsuitability for being used as seed crystal.
The invention provides a preparation method of crystal seeds for treating brushing water, which creatively uses ferrous sulfate to prepare ferroferric oxide crystal seeds by in-situ synthesis under the normal temperature condition, and has the characteristics of amorphous shape, defects of crystal lattices, fine particles, good dispersibility and strong activity. The material used for preparing the seed crystal is pure, no other pollutant is brought in, the seed crystal is prepared at normal temperature, the reaction time is short, the energy consumption required by heating is avoided, and the preparation cost is low.
The invention can be well connected with the existing pickling process and the pickling waste liquid treatment process, the prepared ferroferric oxide crystal seed can efficiently remove metal ions in the scrubbing water in the implementation application, in the scrubbing water system, the crystal seed becomes an external crystal nucleus in the scrubbing water, iron ions and chromium ions in the water tend to attach the crystal nucleus to crystallize and grow into crystal grains, sodium hydroxide is added to adjust the pH value, nickel becomes nickel hydroxide to be coprecipitated with the crystal grain-formed spinel containing ferrochrome, the solid obtained after filtration is the nickel-chromium-iron crystal ore, and the cost of a reducing agent and a flocculating agent is saved. The seed crystal prepared by the invention does not generate acid mud in application, so that the cost for reprocessing the acid mud is saved; and when the seed crystal is used for treating the washing water, the total metal grade of the induced precipitate is high, the regenerated water is not polluted, and the recovered regenerated water and the nickel-chromium-iron crystal ore are valuable and have positive benefits.
Detailed Description
The technical solution of the present invention can be specifically implemented as follows.
The preparation method of the crystal seed for treating the brushing water comprises the following steps:
a. preparing or preparing a solution containing ferrous ions;
b. adding a pH regulator into the solution obtained in the step a, and regulating the pH of the solution to be 8-9 stably;
c. b, adding a transforming agent into the solution obtained in the step b until the solution is changed from blue green to black;
d. and d, standing and aging the solution obtained in the step c to obtain a seed crystal liquid containing ferroferric oxide seed crystals.
In the step a, other substances in the solution containing ferrous ions do not influence the subsequent generation of the ferroferric oxide crystal seeds.
Preferably, the solution containing ferrous ions in step a is a prepared or prepared ferrous sulfate solution, the ferrous sulfate solution may be a prepared or purchased pure ferrous sulfate solution, or other ferrous sulfate industrial waste materials, such as ferrous sulfate waste residues obtained in a titanium dioxide process, may also be used, but it is understood by those skilled in the art that other substances in the solution should not affect the subsequent generation of ferroferric oxide seed crystals. Because the solid ferrous sulfate has wide sources, low price, convenient transportation and no other pollutants, the ferrous sulfate is preferably used as the raw material to prepare the ferrous sulfate solution in the technical scheme of the invention.
The prepared ferrous sulfate solution has too high concentration, which can influence the color observation in the subsequent reaction; the concentration is too low, too much water is introduced for effect in use, so it is preferable that the concentration of the ferrous sulfate solution prepared in step a is 20-25%.
In the step b, the pH regulator refers to at least one of sodium carbonate and sodium hydroxide, the pH regulator is used for regulating the pH of the reaction system, and the sodium hydroxide does not generate carbon dioxide gas to escape in the reaction process, so the sodium hydroxide is preferably used as the pH regulator in the technical scheme of the invention.
In order to save cost and improve reaction efficiency, it is preferable that the pH adjuster is a sodium hydroxide solution having a concentration of 25 to 35%.
In the step c, the transforming agent is at least one of oxygen, air and hydrogen peroxide, and has the function of transforming ferrous iron into ferric iron, and hydrogen peroxide participates in the reaction at a high speed, and the reaction end point is easy to control, so hydrogen peroxide is preferably used as the transforming agent in the technical scheme of the invention.
In order to accelerate the reaction rate and make the reaction more complete, it is preferred that both steps b and c, above, are carried out under stirring.
And d, filtering the seed crystal liquid obtained in the step d to obtain ferroferric oxide seed crystals.
The prior magnetite taking ferroferric oxide as a main component and the ferroferric oxide generated by taking ferric oxide as a batch material cannot be used as seed crystals due to complete crystallization and low activity. The ferroferric oxide seed crystal prepared by the invention is prepared by utilizing the ferroferric oxide seed crystal synthesized in situ by ferrous iron, wherein the in-situ synthesis means that the ferric oxide required for generating the ferroferric oxide is not from an additive but is generated by oxidizing the ferrous oxide in a ferrous oxide system in a ferrous oxide single composition system, so the prepared seed crystal has the characteristic of amorphous shape, and the crystal lattice has defects, high activity, fine particles and easy dispersion.
The technical solution and effects of the present invention will be further described below by way of practical examples.
Examples
100g of ferrous sulfate was added to 400ml of water, and the solution was dissolved with stirring at pH5.5, and the pH was adjusted to 8 with 30% sodium hydroxide while stirring. And then, adding hydrogen peroxide into the solution intermittently and slowly, wherein the intermittent addition of hydrogen peroxide means that the color of the liquid surface turns red instantly when the hydrogen peroxide is added into the solution, which indicates that ferrous iron is converted into ferric iron, at the moment, the addition of hydrogen peroxide is stopped, the red liquid reacts with the blue-green ferrous mother solution under the stirring condition, the surface red disappears, and hydrogen peroxide is added, and the operation is repeated until the color of the solution is changed from blue green to black. Stopping stirring, standing for 2 hours, and then obtaining precipitated solid which is ferroferric oxide seed crystal, and stirring uniformly when in use, wherein the obtained solution is ferroferric oxide liquid crystal.
In this embodiment, three groups of application effects of treating the brushing water by using the liquid ferroferric oxide crystal prepared by the present invention are provided, for example, in examples 1, 2 and 3, 5000ml of brushing water is taken from example 1 and 2, and 10000ml of brushing water is taken from example 3, and the results of detecting the water quality are shown in table 1.
TABLE 1 Water quality test results for brushing Water
| Examples of the invention | pH | turbidity/mg/L | hardness/mg/L | Fe/mg/L | Cr/mg/L | Ni/mg/L |
| 1 | 4 | 17.6 | 200 | 209 | 0.14 | 15 |
| 2 | 5.5 | 3.5 | 50 | 108 | 0.33 | 4.4 |
| 3 | 3 | 22 | 184 | 310 | 88.2 | 95 |
Example 1 after adding 50ml of the prepared ferroferric oxide liquid crystal to brushing water and stirring for 2 minutes, the pH value is adjusted to 8.5 by 30 percent sodium hydroxide solution, and the stirring is continued for 3 minutes; example 2 adding 35ml of the prepared ferroferric oxide liquid crystal to brushing water, stirring for 2 minutes, adjusting the pH to 8 by using 25% sodium hydroxide solution, and continuing stirring for 2 minutes; example 3 to the brushing water was added 80ml of the above-prepared liquid ferroferric oxide crystals, and after stirring for 5 minutes, the pH was adjusted to 8 with 30% sodium hydroxide solution and stirring was continued for 5 minutes. After the stirring is stopped, sedimentation occurs, the solid-liquid separation is carried out on the reaction liquid, the filtrate is the regenerated water, and the water quality detection result is shown in table 2; the solid was a nicr-fe ore, and its chemical composition was measured after drying as shown in table 3.
TABLE 2 quality test results of treated reclaimed water
| Examples of the invention | pH | turbidity/mg/L | hardness/mg/L | Fe/mg/L | Cr/mg/L | Ni/mg/L |
| 1 | 8.3 | Not detected out | Not detected out | Micro-scale | Not detected out | Not detected out |
| 2 | 8 | Not detected out | Not detected out | 0.34 | Not detected out | 0.2 |
| 3 | 7.8 | 0.46 | Not detected out | Not detected out | 0.01 | Not detected out |
TABLE 3 chemical composition of post-drying NiCrFe-crystallite ore powder (wt.%)
| Examples of the invention | TFe | Cr2O3 | Ni |
| 1 | 45.59 | 2.9 | 2.56 |
| 2 | 45.84 | 4 | 1.7 |
| 3 | 47 | 2 | 2 |
Comparative examples magnetite and ferrous sulfate, which were the main components of ferroferric oxide, and ferroferric oxide, which was prepared using ferric oxide as the raw material, were used as the seed crystals, and after adding the rinse water, the above procedure was performed, and as a result, neither of the two ferroferric oxides was crystallized with the metal ions in the rinse water, nor reacted with the rinse water.
The embodiment and the comparative example show that the ferroferric oxide liquid crystal prepared by the method can efficiently remove metal ions in the brushing water in the implementation and application, and the iron grade of the solid product nickel-chromium-iron crystal ore can reach 45 percent, the chromium grade can reach 4 percent and the nickel grade can reach 2 percent when the brushing water is treated by seed crystal induced crystallization, so that the method has recycling value.
The method for preparing the ferroferric oxide seed crystal at normal temperature has the advantages of short reaction time, no energy consumption required by heating and low preparation cost. The ferroferric oxide crystal seeds prepared by the method and the washing water treated by the crystal seeds can save a large amount of cost, such as: the cost of the medicament, the cost of hazardous waste disposal and the like can reduce the total cost; recovering nickel-chromium-iron crystal ore and obtaining positive income; the ferroferric oxide crystal seed induced crystallization reaction speed is high, so that the method is suitable for large-scale drainage during treatment of brushing water; the treatment equipment is the universal equipment in the prior art, the occupied area is small, and the required investment is low.
Claims (9)
1. The preparation method of the crystal seed for treating the brushing water is characterized by comprising the following steps:
a. preparing or preparing a solution containing ferrous ions;
b. adding a pH regulator into the solution obtained in the step a, and regulating the pH of the solution to be 8-9 stably;
c. b, adding a transforming agent into the solution obtained in the step b until the solution is changed from blue green to black;
d. and d, standing and aging the solution obtained in the step c to obtain a seed crystal liquid containing ferroferric oxide seed crystals.
2. The method of preparing a seed crystal for treating a washing water according to claim 1, characterized in that: in the step a, the solution containing ferrous ions is a ferrous sulfate solution.
3. The method of preparing seed crystals for treating brushing water according to claim 2, characterized in that: the concentration of the ferrous sulfate solution is 20-25%.
4. The method of preparing a seed crystal for treating a washing water according to claim 1, characterized in that: in the step b, the pH regulator is at least one of sodium carbonate and sodium hydroxide.
5. The method of preparing seed crystals for treating washing water according to claim 4, wherein: the pH regulator is 25-35% sodium hydroxide solution.
6. The method of preparing a seed crystal for treating a washing water according to claim 1, characterized in that: in step c, the converting agent is at least one of oxygen, air and hydrogen peroxide.
7. The method of preparing a seed crystal for treating a washing water according to claim 1, characterized in that: and c, performing the steps b and c under the stirring condition.
8. The method of preparing a seed crystal for treating a washing water according to claim 1, characterized in that: and d, filtering the seed crystal liquid obtained in the step d to obtain ferroferric oxide seed crystals.
9. The method of producing seed crystals for treating brushing water according to any one of claims 1 to 8, characterized in that: the ferroferric oxide crystal seed is synthesized in situ by ferrous iron, and is amorphous, and has crystal defects and high reaction activity.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011502700.2A CN112499690A (en) | 2020-12-17 | 2020-12-17 | Preparation method of crystal seed for treating brushing water |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011502700.2A CN112499690A (en) | 2020-12-17 | 2020-12-17 | Preparation method of crystal seed for treating brushing water |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807262A (en) * | 2006-02-13 | 2006-07-26 | 上海一品颜料有限公司 | Method for preparing ferriferrous oxide black pigment |
| CN109665566A (en) * | 2019-01-23 | 2019-04-23 | 深圳市长隆科技有限公司 | A kind of preparation method and sewage water treatment method of magnetic nano ferroferric oxide |
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2020
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| CN1807262A (en) * | 2006-02-13 | 2006-07-26 | 上海一品颜料有限公司 | Method for preparing ferriferrous oxide black pigment |
| CN109665566A (en) * | 2019-01-23 | 2019-04-23 | 深圳市长隆科技有限公司 | A kind of preparation method and sewage water treatment method of magnetic nano ferroferric oxide |
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