CN109534472A - A kind of recycling and reuse method of polishing powder from rare earth waste material - Google Patents
A kind of recycling and reuse method of polishing powder from rare earth waste material Download PDFInfo
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- CN109534472A CN109534472A CN201910067961.7A CN201910067961A CN109534472A CN 109534472 A CN109534472 A CN 109534472A CN 201910067961 A CN201910067961 A CN 201910067961A CN 109534472 A CN109534472 A CN 109534472A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of recycling and reuse methods of polishing powder from rare earth waste material, include the following steps: (1) by polishing powder from rare earth waste material and mixed in hydrochloric acid acidleach, when mixed liquor is dissolved completely in the lye that pH is 11~13 without muddiness, acid-leaching reaction is reached home, and acid leaching residue and filtrate are filtered to obtain；(2) H is used2O2Filter residue and washing lotion are obtained after washing to acid leaching residue；(3) washing lotion in the filtrate and step (2) in step (1) is mixed up to composite coagulant.A kind of composite coagulant at low cost, environmental-friendly, simple process, the generation without " three wastes " has been made using polishing powder from rare earth waste material as raw material in this method.
Description
Technical field
The invention belongs to polishing powder from rare earth technical field of waste recovery, it is related to a kind of recycling and again of polishing powder from rare earth waste material
Using method, in particular to a kind of composite coagulant prepared by polishing powder from rare earth waste material and its answering in the treatment of waste water
With.
Background technique
Polishing powder from rare earth is the significant surfaces finishing grinding-material of mobile phone touch glass panel, panel display screen manufacture.
Polishing powder from rare earth then becomes polishing powder from rare earth waste material after using failure.
According to incompletely statistics, currently, domestic polishing powder from rare earth waste material annual output is up to 200,000 tons (butt) Zuo Yous, and be averaged with
Annual 15% or more speed increases.By taking the scientific & technical corporation of Changsha as an example, major product is handset viewing window protective glass, touch screen glass
Glass panel, touch function glass panel, 3D bend glass, touch function glass panel, TFT-LCD, PDP, OLED, FED plate
Display screen, 3D display screen and display screen material etc..Failed polishing powder is rare earth during these product surface finishing polishes
Polishing powder waste material.Scientific & technical corporation's polishing powder from rare earth amount of waste is about 28000 tons (butts) within 2015, reaches 35000 within 2017
Ton (butt), then reaches 40000 tons (butts) or more for 2018.
These waste materials, which are substantially all, to be landfilled or is stored up as solid waste, and the wasting of resources is extremely serious, and there is safety
Hidden danger.Though there are some research reports about it for the purpose of Extraction of rare earth element, industrialization is not implemented.Using chemical method
When, the problem of there is also process flow length, high production cost, operating environment difference etc., (Huang Yaqin, Fu Jie, Jiang Kun etc. were discarded
The comprehensive utilization of polishing powder from rare earth is summarized, it is resource-effective with it is environmentally friendly, 2018, (1): 70,79).Yang Qingshan, Xie Shengzhong, Xu Tuo etc.
(polishing powder from rare earth waste regeneration utilization experimental study, rare metal and hard alloy, 2018,46 (3): 43~45), it has been reported that
Low-temperature decomposition polishing powder from rare earth waste material, successively through drying, acidleach, removal of impurities, precipitating, filtering, roasting and etc. superfinishing is prepared
Close polishing powder from rare earth.But the process flow is complicated, energy consumption is high, and a large amount of exhaust gas, waste water and waste residue is successively discharged etc., and
The hydrofluoric acid raw material etc. of severe toxicity is also used in production process.
Summary of the invention
Aiming at the problems existing in the prior art, returning the object of the present invention is to provide a kind of polishing powder from rare earth waste material
It receives and reuse method, this method has been made a kind of at low cost, environmental-friendly compound using polishing powder from rare earth waste material as raw material
Coagulant, simple process, the generation without " three wastes ".
To achieve the goals above, the present invention provides a kind of recycling and reuse method of polishing powder from rare earth waste material, packets
Include following steps:
(1) by polishing powder from rare earth waste material and mixed in hydrochloric acid acidleach, when mixed liquor is dissolved completely in the lye that pH is 11~13
In without muddiness when, acid-leaching reaction is reached home, and acid leaching residue and filtrate are filtered to obtain；
(2) H is used2O2Filter residue and washing lotion are obtained after washing to acid leaching residue；
(3) washing lotion in the filtrate and step (2) in step (1) is mixed up to composite coagulant.
Preferably, the hydrochloric acid is mass fraction >=31wt% technical grade concentrated hydrochloric acid, and concentrated hydrochloric acid additive amount is rare earth throwing
Light powder metals from waste ion conversion is 1.01~1.05 times of the theoretical amount of chloride.
Preferably, the acidleach temperature is 105~115 DEG C.
Preferably, the lye is selected from least one of sodium hydroxide, potassium hydroxide and ammonium hydroxide.
Preferably, the H2O2Mass fraction be 3~5wt%, H2O2Additive amount be polishing powder from rare earth waste material in Ce3+
It is converted into Ce4+2~3 times of theoretical amount.
Preferably, metallic element leaching rate >=99.9% in the filter residue.
The present invention also provides the applications of composite coagulant prepared by the above method, are used at heavy metal wastewater thereby
Reason.
Basic principle of the invention are as follows:
It is that following acid-leaching reaction occurs under heating for polishing powder from rare earth waste material and hydrochloric acid first:
Al2O3+ 6HCl=2AlCl3+3H2O (1)
Fe2O3+ 6HCl=2FeCl3+3H2O (2)
2CeO2+ 8HCl=2CeCl3+Cl2+H2O (3)
La2O3+ 6HCl=2LaCl3+3H2O (4)
CaO+2HCl=CaCl2+H2O (5)
Na2O+2HCl=2NaCl+H2O (6)
K2O+2HCl=2KCl+H2O (7)
MgO+2HCl=MgCl2+H2O (8)
F-+ HCl=HF+Cl- (9)
After acid-leaching reaction, Al2O3And Fe2O3Form respectively traditional AlCl3And FeCl3Coagulant, and CeO2And
La2O3Then foring has than AlCl3And FeCl3More preferable performance is (because of rare earth element ce3+And La3+With than Al3+And Fe3+More
Hydroxyl bridge linking effect needed for strong coagulation) novel coagulant CeCl3And LaCl3。
In above-mentioned acid-leaching reaction, a small amount of Cl as caused by formula (3)2Can be soluble in water immediately and generate corresponding hydrochloric acid
And hypochlorous acid (because system is in acidity), and the minute quantity HF as caused by formula (9) also can be dissolved in immediately water and be conducive to rare earth
The acid-leaching reaction of element.Therefore, acid-leaching reaction process will not generate new environmental pollution.
After the completion of acid-leaching reaction, into filtering.Filtered acid leaching residue, using 3~5wt%H2O2Solution elution, by acidleach
Remaining a small amount of effective component is washed till 3~5wt%H on slag2O2In washing lotion, elution and the filter residue after draining then can be through further
Processing is prepared into ultra-fine SiO2Powder.
Finally, filtered filtrate, with 3~5wt%H2O2Following oxidation occurs under mildly acidic conditions for washing lotion mixing also
Original reaction:
2Ce3++H2O2+2H+=2Ce4++2H2O (10)
According to Schulze-Hardy rule, cohesiveness is directly proportional to six powers of charge, Ce3+It is oxidized to stable Ce4+
After, corresponding coagulability rises to original 5~6 times.
As described above, efficient composite coagulant is just prepared: both containing traditional Al3+And Fe3+, and containing new
The Ce of type4+And La3+。
Beneficial effects of the present invention:
(1) atom utilization is high and versus environmental is friendly
Polishing powder from rare earth waste material prepares composite coagulant, acid-leaching reaction metallic element leaching rate can reach 99.9% with
On, wherein A13+、Ce4+、La3+And Fe3+Deng all acting as coagulant, trace heavy metal element Ni2+、Zn2+、Cu2+、Cr3+、Pb2+、
Cd2+And Hg2+Deng, it may act as coprecipitated dose of metal that can further enhance treatment effect in heavy metal containing wastewater treatment, and other are golden
Belong to Elements C a2+、Mg2+、Na+、K+Deng, then because compression double electric layer needed for being conducive to coagulation can serve as flocculation aid to a certain extent,
Atom utilization is high.The SiO in filter residue is entered after acidleach and filtering2, further processed high added value can be prepared
Ultra-fine SiO2Powder.
Meanwhile using the preparation method, on the one hand, it is anti-that polishing powder from rare earth waste material can direct plunge into acidleach without dry
It answers, almost without exhaust gas generation；On the other hand, the technical process such as acid-leaching reaction, filtering, elution and mixing will not nearly all be brought
New environmental pollution.Moreover, obtained coagulant is applied to wastewater treatment, it can accomplish " treatment of wastes with processes of wastes against one another ".
Therefore, polishing powder from rare earth waste material prepares composite coagulant, and atom utilization is high and versus environmental is friendly.
(2) process flow is simple and operation is of less demanding
Polishing powder from rare earth waste material prepares composite coagulant, need to only form by acid-leaching reaction, filtering and three steps of mixing, work
Skill is simple, mild condition.Wherein, acid-leaching reaction only need to be leached once.Meanwhile being different from existing by metal in measurement reaction solution
Constituent content judges terminal, and analysis result seriously lags, moreover, the reaction time too long often leads to metallic element leaching rate
Decline instead；When acidleach mixed liquor is dissolved completely in the lye that pH is 11~13 without muddiness by the present invention, it is determined as acidleach
Reaction is reached home, and method is simple, quick, accurate, the metal element contents such as contained Al, Fe, Ce, La in filtrate product and filter residue
Analysis and pilot scale reaction front and back mass balance the result shows that, metallic element leaching rate can reach 99.9% or more.
Therefore, polishing powder from rare earth waste material prepares composite coagulant, and process flow is simple and operation is of less demanding, is easy to full
Sufficient industrialization production requirements.
(3) production cost is low and coagulation performance is excellent
Polishing powder from rare earth waste material prepares composite coagulant, by technical grade concentrated hydrochloric acid price and disposition polishing powder from rare earth waste material
Gained income etc. is all taken into account, and by existing market market, the cost of raw material for producing composite coagulant is much smaller than zero, synthesis
Consider cost of labor, investment recycling and equipment depreciation etc., production run is at low cost.
Since compound coagulant contains Al simultaneously3+、Ce4+、La3+、Fe3+Etc. a variety of high-valence cationics, especially Ce4+, tool
The effect of compression double electric layer needed for having significant coagulation, moreover, rare earth element ce4+、La3+With more traditional coagulant Al3+And
Fe3+Hydroxyl bridge linking effect needed for stronger coagulation is very beneficial for being formed the inorganic polymer condensation polymer of more high price, thus,
While further increasing compression double electric layer effect, extraordinary adsorption bridging coagulation can be also obtained.Meanwhile it is compound mixed
Also contain lot of trace heavy metal ion Zn in solidifying agent2+、Cu2+、Cr2+、Pb2+、Cd2+And Hg2+Deng, can with heavy metal in waste water from
Son is co-precipitated.Therefore, which can obtain unexpected processing when being applied to heavy metal containing wastewater treatment
Effect meets current heavy metal containing wastewater treatment urgent need and proposes target requirement very much.
In conclusion polishing powder from rare earth waste material prepares composite coagulant, production cost is low, and coagulation performance is excellent, non-
Often meet current market demand.
Detailed description of the invention
Fig. 1 is the recycling and reuse method and process general flow chart of polishing powder from rare earth waste material；
Fig. 2 is certain heavy metal waste water treatment process general flow chart.
Specific embodiment
By taking the polishing powder from rare earth waste material of Changsha scientific & technical corporation as an example, solid content 57.6wt%, in butt typical case at
Divide such as the following table 1.
Table 1 polishing powder from rare earth waste material (butt) constituent analysis list
| Substance | Content (wt%) | Substance | Content (wt%) |
| Aluminum oxide | 22.05 | Fluoride | 0.11 |
| Silica | 55.08 | Phosphorus pentoxide | 1.35 |
| Di-iron trioxide | 2.31 | Nickel | 2.21×10-4 |
| Ceria | 8.06 | Zinc | 1.27×10-3 |
| Lanthanum sesquioxide | 3.98 | Copper | 7.48×10-4 |
| Calcium oxide | 2.21 | Chromium | 2.34×10-4 |
| Sodium oxide molybdena | 1.44 | Arsenic | 5.55×10-5 |
| Potassium oxide | 0.11 | Lead | 1.39×10-4 |
| Sulfate radical | 0.79 | Cadmium | 2.76×10-5 |
| Chloride | 0.15 | Mercury | 5.54×10-6 |
| Magnesia | 0.54 |
Embodiment 1
By the stoichiometric that above-mentioned chemical equation (1)~(9) provide, hydrochloric acid excess coefficient takes 0.15, respectively plus
Enter polishing powder from rare earth waste material 150g and the 31wt% technical grade of for example above-mentioned table 1 of solid content 57.6wt%, butt ingredient and its content
Concentrated hydrochloric acid 212g, under stiring temperature reaction, temperature control are 105 DEG C of back flow reactions, and fixed time interval takes 1~2 in reaction process
Reaction suspension is dripped, when it can be dissolved completely in the NaOH solution that pH is 11~13 without muddiness, that is, can be shown that acidleach is anti-
It should reach home.
When natural cooling is down to 40 DEG C or less under stiring, filtering can be transferred to.Filtered acid leaching residue, it is pre- using 50g
First configured 3wt%H2O2Solution elution.Wherein H2O2Amount, according to 2 times of above-mentioned reaction equation (10) theoretical amount
It determines.Finally, 3wt%H2O2Washing lotion is incorporated to filtered filtrate, has just obtained composite coagulant target product I.
Product I appearance is rufous transparency liquid, density 1.3kg/L or so, 1wt% aqueous solution pH=2, by oxide
(Al2O3+Fe2O3+CeO2+La2O3) total amount meter, effective content is 10wt% or so.Its coagulation performance evaluation result such as table 2.
Embodiment 2
By the stoichiometric that above-mentioned chemical equation (1)~(9) provide, hydrochloric acid excess coefficient takes 0.01, respectively plus
Enter polishing powder from rare earth waste material 150g and the 31wt% technical grade of for example above-mentioned table 1 of solid content 57.6wt%, butt ingredient and its content
Concentrated hydrochloric acid 186g, under stiring temperature reaction, temperature control are 115 DEG C of back flow reactions, and fixed time interval takes 1~2 in reaction process
Reaction suspension is dripped, when it can be dissolved completely in the NaOH solution that pH is 11~13 without muddiness, that is, can be shown that acidleach is anti-
It should reach home.
When natural cooling is down to 40 DEG C or less under stiring, filtering can be transferred to.Filtered acid leaching residue, it is pre- using 75g
First configured 3wt%H2O2Solution elution.Wherein H2O2Amount, according to 3 times of above-mentioned reaction equation (10) theoretical amount
It determines.Finally, 3wt%H2O2Washing lotion is incorporated to filtered filtrate, has just obtained composite coagulant target product II.
Product II appearance is rufous transparency liquid, density 1.29kg/L or so, 1wt% aqueous solution pH=4, by oxide
(Al2O3+Fe2O3+CeO2+La2O3) total amount meter, effective content is 9.8wt% or so.Its coagulation performance evaluation result such as table 2.
Embodiment 3
By the stoichiometric that above-mentioned chemical equation (1)~(9) provide, hydrochloric acid excess coefficient takes 0.05, respectively plus
Enter polishing powder from rare earth waste material 150g and the 31wt% technical grade of for example above-mentioned table 1 of solid content 57.6wt%, butt ingredient and its content
Concentrated hydrochloric acid 193g, under stiring temperature reaction, temperature control are 111 DEG C of back flow reactions, and fixed time interval takes 1~2 in reaction process
Reaction suspension is dripped, when it can be dissolved completely in the NaOH solution that pH is 11~13 without muddiness, that is, can be shown that acidleach is anti-
It should reach home.
When natural cooling is down to 40 DEG C or less under stiring, filtering can be transferred to.Filtered acid leaching residue, using 62.5g
Pre-configured 3wt%H2O2Solution elution.Wherein H2O2Amount, according to above-mentioned reaction equation (10) theoretical amount
2.5 times of determinations.Finally, 3wt%H2O2Washing lotion is incorporated to filtered filtrate, has just obtained composite coagulant target product III.
Product III appearance is rufous transparency liquid, density 1.31kg/L or so, 1wt% aqueous solution pH=3, by oxidation
Object (Al2O3+Fe2O3+CeO2+La2O3) total amount meter, effective content is 10.2wt% or so.Its coagulation performance evaluation result is such as
Table 2.
The application of composite coagulant in the treatment of waste water:
Certain heavy metal wastewater thereby, water are 100~110m3/ d, total Ni content 80~90mg/L, pH are 4~5.It is previous to require
Total Ni content is discharged after processing to reach specified in GB8978-1996 no more than 1.0mg/L.Its processing technological flow such as Fig. 2.
Since the waste water is closer from Xiang River main stream, since 2018, Hunan Province's provincial standard (referred to as saves terrestrial reference, similarly hereinafter)
It is required that the total Ni content≤0.2mg/L of water outlet.For this purpose, production manufacturer was added once in adding Na in coagulating basin2S solution (so as to
Form NiS precipitating), in adding the multinomial measure such as DTCR heavy metal chelant in flocculation basin, but be discharged total Ni content and be still up to 0.3
~0.5mg/L, and medicament is costly.
Recently, test changes at neutralization pond front pump outlet conduit (as represented by the arrows in the dashed line in figure 2), adds the present invention and mentions
Composite coagulant out, 400~600mg/L of dosage.Test result drops with being discharged total Ni content immediate stability after showing processing
To 0.1mg/L hereinafter, fully meeting the requirement of total Ni content≤0.2mg/L of province's terrestrial reference proposition.Moreover, coagulant PAC (polymerization
Aluminium chloride) dosage is down to only original 1/10.Total medicament expense, not only without increasing because composite coagulant is added, instead
And it also significantly reduces.It also found contained heavy metal element in compound coagulant simultaneously, after wastewater treatment in water outlet all never
Detection, they are entered in sludge to be processed together with heavy metal in waste water Ni co-precipitation.
Composite coagulant performance evaluation:
Above-mentioned heavy metal wastewater thereby water sample about 1000mL is taken out, Ni content 86mg/L, pH are 4~5, molten using 30wt%NaOH
After liquid stirring neutralizes, it is quickly added with stirring addition 5mg/L dosage PAM (poly- third under a certain amount of composite coagulant, moderate-speed mixer
Acrylamide) flocculant, lower reaction 10min is then mixed slowly again.It is sequentially completed quick mixing, middling speed flocculation and slow reaction
Afterwards, quiescent setting 20min finally takes out the content of supernatant measurement heavy metal Ni respectively again.The results are shown in Table 2:
The coagulation evaluation result of 2 composite coagulant of table
* only PAM dosage is respectively 1500~1600mg/L and 30mg/L to production scene PAC.
As can be seen from Table 2, the PAC and its dosage that use according to production scene, total Ni content can only in water outlet after wastewater treatment
Reach the requirement no more than 1.0mg/L.And composite coagulant proposed by the present invention is used, dosage only 400~600mg/L, just
It can be controlled in the requirement that total Ni content≤0.2mg/L of province's terrestrial reference proposition is fully met no more than 0.10mg/L.
Claims (7)
1. a kind of recycling and reuse method of polishing powder from rare earth waste material, includes the following steps:
(1) by polishing powder from rare earth waste material and mixed in hydrochloric acid acidleach, be dissolved completely in the lye that pH is 11~13 when mixed liquor and
When not muddy, acid-leaching reaction is reached home, and filters to obtain acid leaching residue and filtrate；
(2) H is used2O2Filter residue and washing lotion are obtained after washing to acid leaching residue；
(3) washing lotion in the filtrate and step (2) in step (1) is mixed up to composite coagulant.
2. recycling and reuse method according to claim 1, it is characterised in that: the hydrochloric acid be mass fraction >=
The technical grade concentrated hydrochloric acid of 31wt%, concentrated hydrochloric acid additive amount are the theory that polishing powder from rare earth metals from waste ion conversion is chloride
1.01~1.05 times of amount.
3. recycling and reuse method according to claim 1, it is characterised in that: the acidleach temperature is 105~115
℃。
4. recycling and reuse method according to claim 1, it is characterised in that: the lye is selected from sodium hydroxide, hydrogen
At least one of potassium oxide and ammonium hydroxide.
5. recycling and reuse method according to claim 1, it is characterised in that: the H2O2Mass fraction be 3~
5wt%, H2O2Additive amount be polishing powder from rare earth waste material in Ce3+It is converted into Ce4+2~3 times of theoretical amount.
6. recycling and reuse method according to claim 1, it is characterised in that: metallic element leaching rate in the filter residue
>=99.9%.
7. the application of composite coagulant described in any one of claims 1-6, it is characterised in that: be used for heavy metal wastewater thereby
Processing.
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| CN110241309A (en) * | 2019-05-08 | 2019-09-17 | 湖南景翌湘台环保高新技术开发有限公司 | A kind of method that useless polishing powder from rare earth extracts white carbon black and rare earth water purification agent |
| CN111039495A (en) * | 2020-01-06 | 2020-04-21 | 湖南景翌湘台环保高新技术开发有限公司 | Comprehensive recovery method of waste rare earth polishing powder and steel pickling waste liquid |
| WO2023112046A1 (en) * | 2021-12-17 | 2023-06-22 | Saint-Gobain Glass France | A descaling composition for glass substrates |
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| WO2023112046A1 (en) * | 2021-12-17 | 2023-06-22 | Saint-Gobain Glass France | A descaling composition for glass substrates |
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