Method for integrated treatment of industrial waste water formed when producing extra-pure quartz concentrate

FIELD: chemistry.

SUBSTANCE: invention can be used in production of extra-pure quartz concentrate which is one of the main sources of contamination by fluorine, chlorine and salts containing fluorine and chlorine. The method is realised via reactant treatment in two steps. The first step involves neutralisation of acidic waste water with 23% NH4OH with separation of the SiO2 precipitate and formation of NH4F solution. At the second step, said solution is treated with 20% lime milk. The formed CaF2 precipitate and previously separated SiO2 precipitate are washed, dehydrated and removed from the process as end products. The 7-8% NH4OH solution obtained after separating the CaF2 precipitate and flush water are returned to the first step for reactant treatment of waste water to prepare the starting NH4OH solution. The 7-8% NH4OH solution formed at the second step is concentrated by evaporation to 23% and returned to the first reactant treatment step. The condensate obtained during evaporation is directed for preparation of 20% lime milk, washing the SiO2 precipitate and into recycling cycle of the main production.

EFFECT: invention enables to cut the volume of discharge of industrial wastes into the environment, prevents formation of non-recyclable sludge and also reduces consumption of fresh water during production and enables to obtain high-quality products used in different industries.

3 cl, 1 ex

 

The invention relates to the protection of the environment and can be used in the production of high-purity quartz concentrate, which is one of the main sources of pollution by fluorine, chlorine and salts containing them.

Global consumption of high-purity quartz concentrate annually increases by 8-10% and now makes up more than 50 thousand tons. Meeting the growing needs of high-purity quartz concentrate producers of high-quality raw materials for the electronics industry unfortunately is accompanied by an increase in the volume of industrial wastewater needing cleanup inexpensive but effective ways.

Production of high-purity quartz concentrate produced in the form of quartz grains, powder and powder includes multi-stage technological process of processing of quartz raw materials (ore): crushing, grinding, scrubbing, washing quartz concentrate, screening, filtration, leaching, which consists in the chemical processing of quartz 20-23%hydrofluoric and hydrochloric acids, as well as multiple (up to 10 times) washing with deionized water enriched (Vasilchenko) quartz concentrate, classification, drying at temperatures up to 250°C and calcining at 1200-1600°C. as a result of such processing quartz forms which I am very a large number of acidic industrial effluents, as for processing 1 ton of SiO2up to 12 tons of water. The resultant waste water containing up to 8-26% H2SiF6, 1-3% HF, 1-2% HCl. Therefore, in the production of high-purity quartz concentrate the question about the disposal of these acidic waste, destructive sewer pipe and contaminating the underground water and rivers.

For the treatment of industrial wastewater contained hydrofluoric (HF), kremneftoristogo (H2SiF6) and hydrochloric (HCl) acids and their salts using different methods: ion exchange, sorption, chemical, and electrochemical desalination by reverse osmosis. However, these methods are mainly used for purification of industrial wastewater containing small amounts of fluorine or chlorine to the target value of MPC or MPD.

Known reagent purification method of fluorine-containing waste water (SU 1171433 And 07.08.1985). This method relates to the treatment of industrial effluents, which contain a small amount of fluoride (up to 10 g/l). The method consists in the neutralization of acidic waste calcium-containing reagent, such as calcium hydroxide CA(Oh)2(milk of lime). Formed in the process of cleaning the precipitate of calcium fluoride (fluorite) is filtered and washed, and the filtrate and the washing water is neutralized.

The main disadvantage of Izvestkovaya is the impossibility of its application for the purification of acidic industrial effluents, formed in the production of high-purity quartz concentrate and contain large amounts of fluorine and SiO2. In addition, in a known way to produce large quantities of acidic waste requiring additional neutralization, and because of its high content in sediment slurry of silicon oxide quality metallurgical fluorite from it.

The closest in technical essence and the achieved result is a method of chemical treatment of industrial wastewater containing a large amount of fluoride (up to several hundred g/l solution). The method consists in the neutralization of acidic waste suspension of chalk (caso3and/or hydroxide CA(OH)2in the form of lime milk (Vasilev, AA Novikov, Wearden. "Production of fluorine compounds during the processing of phosphate raw materials", Moscow, Chemistry, 1982, s).

Implement the method as follows. Industrial effluents after the leaching of quartz concentrate hydrofluoric acid and rinsing with deionized water, dilute with water to obtain a 1%solution of H2SiF6that is loaded into the reactor. Then, the reactor serves pre-cooked "milk of lime". The neutralization process lead to pH 10-12, and for completeness of the reaction of introducing an excess of Cao (8-10% higher than required is depending on stoichiometry). To expedite the preparation of neutralizing agent used "milk of lime" high concentration (20%). The neutralization process is conducted for 1 hour at pH 10-12 and under vigorous stirring. At the end of the neutralization process is provided by the introduction of flocculants. The use of flocculants is necessary to reduce sedimentation, reduce the amount of generated sludge and acceleration of the process of separation of the solid phase (sludge) from the solution by filtration. After settling the clarified water with a pH of about 8,0-8,5 douchemat one of the above methods to set the values of the MPC or MPD and throw in special pools or rivers, and settled sludge (humidity 75-80%) with flocculants sent to the sludge trap and then sent to be deposited in a special slurry pad.

The main disadvantages of this method are the increased number of acidic waste (up to 4-5 times) by pre-diluting the original industrial waste water to obtain a 1%solution of H2SiF6and the presence of sludge containing acid solutions. Obtained after extraction of sludge from the clarified water and water obtained after filtering, in most cases, clean up MAC from the remnants of salts HF, H2SiF6and HCl is impossible. In addition, sludge and clarified water contain a flocculant is. Therefore, the reuse of such water in the production of high-purity quartz concentrate, since organic substances included in the chamber of the wash water are sorbed on the surface of quartz concentrate, which leads to a significant deterioration of its quality. Due to the high content in the slurry of silicon oxide quality metallurgical fluorite is impossible, as obtained from metallurgical fluorite contains about 40% SiO2and the lowest quality brand metallurgical fluorite used in metallurgy, contains not more than 30% SiO2.

The technical result of the claimed invention is an integrated treatment of industrial wastewater, preventing discharge of industrial effluent into the environment during the production of very pure quartz concentrate, excluding education unusable sludge, a sharp decline in consumption in the production of very pure quartz concentrate fresh water, and receiving from industrial effluent quality of target products, widely used in several industries. In addition, treatment of acidic industrial wastewater the proposed method is carried out without the use of flocculants.

The technical result is achieved by the fact that a comprehensive treatment of industrial the wastewater, formed in the production of high-purity quartz concentrate, perform reagent treatment in two stages, the first stage are wastewater neutralization 23%solution of NH4OH with the release of sediment SiO2and the formation of a solution of NH4F, which is then in the second stage process of 15-20%lime milk, the resultant precipitate CaF2and previously allocated sediment SiO2washed, dewatered and removed from the process as a ready target products, and the resulting 7-8%solution of NH4OH after the precipitate CaF2and rinse water back to the first stage of chemical treatment of wastewater for the preparation of the initial solution of NH4OH.

It is this combination and sequence of methods, reagents and conditions cleaning is necessary to achieve the claimed technical result and provides a comprehensive treatment of industrial wastewater generated in the production of high-purity quartz concentrate.

In a preferred embodiment, the method ammonia water (7-8%solution of NH4OH) after the second stage concentrated by evaporation to obtain 23% of NH4OH and back to the first stage of chemical treatment, and the resulting condensate is used in three ways - making a 15-20%and vescovado milk, the sediment washing SiO2and also send in the working cycle of the primary production of very pure quartz concentrate.

For the release of silica from the remnants of fluorine, chlorine and ammonia, i.e. improve the quality of SiO2received after the last washing SiO2the water sent for treatment on membrane reverse osmosis desalination, where it is cleaned from salts of ammonia, fluorine and chlorine and return to the last rinsing of the silicon dioxide (white carbon black), which after the last washing, dewatered, and then passes through a stage of thermal treatment in the temperature range 110-700°C.

The cleaning process is as follows. In the first stage of chemical treatment of acidic wastewater (industrial wastewater) production of very pure quartz concentrate is loaded into the reactor, where, continuously mixed, they fill the reactor to a certain extent. Then in a reactor for carrying out the process of neutralization serves a 23%aqueous solution of ammonia (NH4OH). Time to neutralize the acids contained in the acidic effluents, 30-40 minutes after the neutralization formed suspension consisting of a solution of NH4F and silicon dioxide, which is directed to filtration on a filter press, where the separation of a solid residue SiO2and solution of NH4F. Hotfile the integration of sediment SiO 2several times concentrated, washed with water, wring out to get 70% (on dry matter) of sludge and is removed from the process. The second reagent treatment is to neutralize 15-20%lime milk 7-8%aqueous solution of ammonium fluoride, obtained after the first chemical treatment of industrial wastewater. Upon completion of the reaction is a slurry consisting of 7-8%-aqueous solution of NH4OH (ammonium hydroxide) and a precipitate of calcium fluoride. The suspension is separated in the centrifuge on calcium fluoride (CaF2) humidity 30-40%, which is in the quality of the finished product direct to the consumer, and the clarified part (7-8%solution of NH4OH) back to the first stage of chemical treatment of wastewater for the preparation of the initial solution of NH4OH, or sent to concentration, for example, by evaporation. The resulting concentrate (23%aqueous solution of ammonia) return to the neutralization of newly admitted acidic waste, which is the first implementation of chemical treatment of industrial wastewater, and the resulting condensate is divided, for example, into three streams: the first is directed to the preparation of milk of lime solution, the second wash SiO2the third stream after ion-exchange treatment of traces of impurities is sent to the main production of high-purity quartz concentrate.

With the purpose of getting high is kachestvennoi white black (SiO 2), i.e. the release of sediment SiO2from the remnants of ammonia, fluorine and chlorine obtained after the last washing SiO2the water sent for treatment on membrane reverse osmosis desalination, where it is cleaned from salts of ammonia, fluorine, chlorine, return to the last (final) wash white soot, which is dehydrated, and then is subjected to heat treatment in the temperature range from 110 to 700°C. During heat treatment (drying) of the filtered sludge SiO2in the temperature range 110-112°C the content of SiO2in white soot is 74-77%, while processing in the temperature range of 650-700°C the content of SiO2in white soot is 95-96%.

Thus, the claimed method of chemical treatment of acidic wastewater generated in the production of high-purity quartz concentrate conducted in two stages that allows you to organize environmentally friendly technology with the exception of the discharge of industrial toxic wastes into the environment, dramatically reduce the consumption of fresh water due to its return (to 95%) in production, to eliminate unusable sludge, requiring the construction and maintenance of storage facilities for waste and provides obtaining products with a high content of the main product (up to 96% SiO2and up to 92% CaF2), which is widely used in various is blastah industry (bus, cosmetic, electrical, electronic, construction, steel, leather, chemical). Besides getting white black and fluorite (CaF2) with a high content of basic components allows to obtain metallurgical fluorite virtually any stamps.

1. The method of complex treatment of industrial wastewater generated in the production of high-purity quartz concentrate implemented reagent treatment, including wastewater neutralization with lime milk, subsequent separation of clarified water and the resulting slurry which is washed and sent for recycling, characterized in that the chemical treatment is carried out in two stages, the first stage are wastewater neutralization 23%solution of NH4OH with the release of sediment SiO2and the formation of a solution of NH4F, which is then in the second stage process of 15-20%lime milk, the resultant precipitate CaF2, and was previously allocated sediment SiO2washed; dewatered and removed from the process as a ready target products, and the resulting 7-8%solution of NH4OH after the precipitate CaF2and rinse water back to the first stage of chemical treatment of wastewater for the preparation of the initial solution of NH4OH.

2. The method of complex treatment of industrial the precise water according to claim 1, characterized in that 7-8%solution of NH4OH after the second stage concentrated by evaporation to 23% and return to the first stage of chemical treatment, and the resulting condensate is directed to the preparation of 20%lime milk, washing the precipitate SiO2a working cycle of primary production.

3. The method of complex industrial wastewater treatment according to claim 1, characterized in that the received after the last washing SiO2the water sent for treatment on membrane reverse osmosis desalination, where it is cleaned from salts of ammonia, fluorine and chlorine, and return to the last washing of the precipitated, which after the last washing, dewatered, and then passes through a stage of thermal treatment in the temperature range 110-700°C.



 

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1 tbl, 1 ex

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