CN105521758A - Application method of crystalline hydrate mineral containing amino groups and hydroxyl groups in treatment of zinc-containing wastewater - Google Patents
Application method of crystalline hydrate mineral containing amino groups and hydroxyl groups in treatment of zinc-containing wastewater Download PDFInfo
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- CN105521758A CN105521758A CN201610066817.8A CN201610066817A CN105521758A CN 105521758 A CN105521758 A CN 105521758A CN 201610066817 A CN201610066817 A CN 201610066817A CN 105521758 A CN105521758 A CN 105521758A
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- Prior art keywords
- zinc
- crystalline hydrate
- application process
- hydroxyl
- amino
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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 an application method of crystalline hydrate mineral containing amino groups and hydroxyl groups in treatment of zinc-containing wastewater. The surface of the crystalline hydrate mineral has rich groups such as amino groups, hydroxyl groups and the like, the groups have negative charges and easily form interfacial force with zinc hydroxide in the wastewater for coprecipitation, so that the sizes of precipitate particles are increased, and further zinc hydroxide is rapidly precipitated in a wastewater treatment system. The application method in treatment of the zinc-containing wastewater is implemented according to the procedure of hydrolysis, mixing, stirring and solid-liquid separation, the pH of the system is adjusted to 6.0-7.0 in the hydrolysis process, and an amino group containing crystalline hydrate mineral preparation is added in the mass ratio of mineral to zinc being (0.5-5.0):1.0 during mixing and stirring. The sedimentation performance of zinc hydroxide in the water treatment process can be remarkably improved, and meanwhile, the zinc concentration of effluent can meet the national emission standard.
Description
Technical field
The present invention relates to a kind of containing the application process of crystalline hydrate mineral in zinc-containing water process that be amino and hydroxyl, dig up mine in coloured industry in particular to these mineral, process in zinc-containing water that ore dressing, smelting, processing and electronics industry produce, belong to field of waste water treatment.
Background technology
Zinc-containing water is from electroplating wastewater, mining, non-ferrous metal metallurgy and part chemical enterprise, the discharge of zinc-containing water has serious harm to health and industrial or agricultural activity, there is the harm such as persistence, toxicity is large, seriously polluted, once can not be biodegradable after entered environment, great majority participate in food chain circulation, and finally accumulate in vivo, destroy organism normal bio metabolic activity, be detrimental to health.
The method of Treatment of Zinc-containing Wastewater can be summarized as chemical method, physical-chemical process, bioanalysis three major types.Wherein chemical method has moderate water-cut stage, sulphide precipitation, the ferrite precipitation method, the barium salt precipitation method, oxidation-reduction method, Powder by Iron Powder, By Bubble-floating Method, electrolysis etc.; Physical-chemical process has ion-exchange, absorption method, solvent extraction, liquid-film method, hyperfiltration and electroosmose process; Bioanalysis is divided into biological adsorption and biogenic sediment.Various method all has its pluses and minuses.Method the most frequently used is at present chemical precipitation method, by adding alkali nertralizer, makes zinc ion in waste water form the less zinc hydroxide precipitation of solubility and reach the object removing zinc.Usual employing soda lime (CaO), calcium hydroxide (Ca (OH)
2) etc. nertralizer, cheap; Or interpolation caustic soda, reinforced easily can remove the zinc ion in waste water fast, technical process is simple, but it is still higher to there is water outlet zinc ion concentration, can not the problem of qualified discharge; And sediment weight is less, settling velocity is slow, moisture content is high.Particularly, zinc hydroxide is in the solution in flocculence, and deposit seed is very tiny, in the liquid phase more difficult precipitation, and under condition of different pH, there is multi-form hydroxyl conjunction complex ion (as Zn (OH)
+, Zn (OH)
4 2-, Zn (OH)
3 -), make only to adopt zinc hydroxide precipitation formal layout zinc-containing water difficulty larger, especially for the zinc-containing water of low concentration (1 ~ 20mg/L), owing to being difficult to form zinc hydroxide precipitation particle, treatment effect is more undesirable.
Summary of the invention
Object of the present invention is exactly based on the not good shortcoming of zinc hydroxide precipitation performance in traditional moderate water-cut stage processing procedure, proposes a kind of containing-NH
3with the application process of crystalline hydrate mineral in zinc-containing water process of-OH.
Contain an application process for the crystalline hydrate mineral of amino and hydroxyl, be added to the water for zinc-containing water process; The described mass ratio containing nitrogen in the crystalline hydrate mineral of amino and hydroxyl is greater than 4%, and the mass ratio of hydrogen is greater than 5%, and the mass ratio of oxygen is 60% ~ 70%, crystalline water molecules number is 4 ~ 12, particle size is 10 ~ 100 μm, and zeta current potential is-5 ~-1mV, and mineral density is 1.4 ~ 2.0g/cm
3.
Described is as follows containing crystalline hydrate mineral synthetic method that is amino and hydroxyl: keeping, under the condition stirred, adding magnesium chloride and sodium hydrogen phosphate solid, NH in ammonium chloride solution
4cl, MgCl
2, Na
2hPO
4molar ratio=2 ~ 4:1 ~ 2:1; Then the rapid NaOH solution of 1mol/L input in the solution system after adding magnesium chloride and sodium hydrogen phosphate is reacted, and is taken out by sediment dry.
The described synthetic method containing the crystalline hydrate mineral of amino and hydroxyl is specific as follows:
1) ammonium chloride solution of 2g/L is prepared in N, according to molar ratio n (NH
4cl): n (MgCl
2): n (Na
2hPO
4)=2 ~ 4:1 ~ 2:1 prepares quantitative magnesium chloride and sodium hydrogen phosphate solid, and prepares the NaOH solution of 1mol/L;
2) keeping under the condition stirred, in the ammonium chloride solution of preparation, adding magnesium chloride and sodium hydrogen phosphate solid, according to volume ratio v (NaOH): v (NH
4cl)=0.01 ~ 0.04:1, drops into the NaOH solution of 1mol/L rapidly in the solution system after adding magnesium chloride and sodium hydrogen phosphate; Maintenance system mixing speed is 400 ~ 600r/min, time 10 ~ 40min;
3) sediment is taken out drying, control baking temperature is 40-50 DEG C, time 2 ~ 6h.
Specifically comprise the following steps during application:
(1) regulate zinc-containing water pH value, make containing zinc ion generation hydrolysis;
(2) in the zinc hydroxide system after hydrolysis, add the crystalline hydrate mineral containing amino and hydroxyl;
(3) solid-liquid system of step (2) gained is carried out leave standstill, Separation of Solid and Liquid.
Step (1) regulates zinc-containing water pH value to 6-7, and reaction time control is 10 ~ 20min.
Step (1) uses the NaOH solution of 1mol/L or lime milk solution to regulate zinc-containing water pH value.
Step (2) is 0.5 ~ 4.0:1.0 containing the mass ratio of zinc in the crystalline hydrate mineral dosage of amino and hydroxyl and system.
Step (2) reaction time is 10 ~ 40min.
Step (2) stir speed (S.S.) controls at 100 ~ 300r/min.
Step (3) time of repose is 10 ~ 20min.
The present invention studies discovery, and some crystalline hydrate mineral particle diameter when just synthesizing is tiny, has larger specific area, has stronger suction-operated; And its surface is not only containing hydroxyl (-OH can be provided by the crystallization water), also containing amino (-NH
3) etc. multiple group, very easily and form the high forces chemical bonds such as hydrogen bond between zinc hydroxide (containing-OH), be conducive to the attachment precipitation of zinc hydroxide; And this hydrated mineral surface is often electronegative, by electrostatic attraction, Electrostatic Absorption occurs with the zinc hydroxide of surface band positive charge.All these can realize the reinforced deposition of zinc hydroxide in zinc-containing water chemical neutralization precipitation process process, thus improves the removal efficiency of zinc-containing water.
Based on above thinking, the present invention searches out a kind of containing amino (-NH
3) and the crystalline hydrate mineral of hydroxyl (-OH), by the interaction between itself and zinc hydroxide interface, the rapid precipitation of zinc hydroxide can be realized and efficiently to remove, for efficient, the advanced treating of zinc-containing water provide feasible technical scheme.
Below in conjunction with the drawings and specific embodiments, the invention will be further described, and unrestricted the present invention.
Accompanying drawing explanation
Fig. 1 is of the present invention containing amino (-NH
3) and the FT-IR collection of illustrative plates of crystalline hydrate mineral of hydroxyl (-OH);
In figure ~ 1436cm
-1the strong absworption peak at place is amino-NH
3the flexural vibrations of middle N-H, ~ 3000cm
-1the wide absworption peak at left and right place is-NH
3the stretching vibration of middle N-H, ~ 1630cm
-1the absworption peak at place is designated as the stretching vibration of hydroxyl-OH.
Fig. 2 is of the present invention containing amino (-NH
3) and the technological process of applying in zinc-containing water process of the crystalline hydrate mineral of hydroxyl (-OH).
Detailed description of the invention
Embodiment 1:
The ammonium chloride solution 3L of preparation 2g/L (N meter), according to n (NH
4cl): n (MgCl
2): n (Na
2hPO
4the molar ratio of)=2:1:1 takes quantitative magnesium chloride and sodium hydrogen phosphate solid, then prepares the NaOH solution of 1mol/L.Keeping under the condition stirred, in the ammonium chloride solution of preparation, adding magnesium chloride and sodium hydrogen phosphate solid, proportionally v (NaOH): v (NH
4cl)=0.0325:1, measures NaOH solution 97.5mL, and the NaOH solution measured is dropped in the system after adding magnesium chloride and sodium hydrogen phosphate rapidly.Mixing speed is adjusted to 500r/min, and mixing time controls as 30min.After Separation of Solid and Liquid, taken out by sediment dry, controlling baking temperature is 50 DEG C, after dry 2h, obtains of the present invention containing amino (-NH
3) and hydroxyl (-OH) crystalline hydrate mineral.
Embodiment 2:
What record embodiment 1 synthesis contains amino (-NH
3) and the crystalline water molecules number of hydroxyl (-OH) crystalline hydrate mineral be 6, mineral averag density is 1.8g/cm
3, nitrogen content is 5.71%, and hydrogen content is 6.5%, oxygen content position 65.3%, and the average grain diameter recording these crystalline hydrate mineral after 30min reaction is 30.2 μm, zeta current potential-2.6mV, and the infared spectrum display of mineral surfaces is wherein containing the amino (-NH of instruction
3), the peak (Fig. 1) of hydroxyl (-OH).
Embodiment 3:
Get the zinc-containing water 1L of zinc concentration 200mg/L, under the state stirred, add caustic soda raising system pH in waste water is 6.0, makes zinc ion generation hydrolysis.Then in the solid-liquid mixed system after hydrolysis, add that embodiment 1 obtains containing crystalline hydrate mineral that are amino and hydroxyl, in its dosage and waste water, the mass ratio of zinc is 2:1.Then mix and blend 30min is carried out.The solid-liquid system of gained is carried out Separation of Solid and Liquid, and recording Zn content in supernatant is 0.02mg/L, reaches " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).Precipitate and detect through particle size analyzer, average particle diameter size reaches 29.5 μm.As a comparison, wastewater sample is adopted traditional alkali adding method process, caustic soda is added in waste water, pH is adjusted to 8.0, and after hydrolysis 30min, detecting Zn content residual in its solution is 10.2mg/L, and its precipitation average grain diameter is 8.1 μm, show the zinc-containing water for higher concentration, adopt method of the present invention can strengthen zinc hydroxide rapid precipitation, and make zinc-containing water result reach discharge standard.
Embodiment 4:
Get the zinc-containing water 1L of zinc concentration 10mg/L, under the state stirred, add caustic soda raising system pH in waste water is 6.0.Then add containing hydroxy amino crystalline hydrate mineral in the solid-liquid mixed system after hydrolysis, its dosage control be: in crystalline hydrate mineral preparation and waste water, the mass ratio of zinc is 5.0:1.Reaction time controls as 20min.The solid-liquid system of gained is carried out Separation of Solid and Liquid, and recording Zn content in supernatant is 0.09mg/L, reaches " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).Precipitate and detect through particle size analyzer, average particle diameter size reaches 19.9 μm.As a comparison, wastewater sample is adopted traditional alkali adding method process, caustic soda is added in waste water, pH is adjusted to 9.0, and after hydrolysis 30min, detecting Zn content residual in its solution is 6.8mg/L, and its precipitation average grain diameter is 2.9 μm, show the zinc-containing water for low concentration, adopt method of the present invention still can strengthen zinc hydroxide rapid precipitation, and make zinc-containing water result reach discharge standard.
Table 1 embodiment 3 and 4 zinc-containing water handling property
Claims (10)
1. contain an application process for the crystalline hydrate mineral of amino and hydroxyl, it is characterized in that, be added to the water for zinc-containing water process; The described mass ratio containing nitrogen in the crystalline hydrate mineral of amino and hydroxyl is greater than 4%, and the mass ratio of hydrogen is greater than 5%, and the mass ratio of oxygen is 60% ~ 70%, crystalline water molecules number is 4 ~ 12, particle size is 10 ~ 100 μm, and zeta current potential is-5 ~-1mV, and mineral density is 1.4 ~ 2.0g/cm
3.
2. application process according to claim 1, is characterized in that, described is as follows containing crystalline hydrate mineral synthetic method that is amino and hydroxyl: keeping, under the condition stirred, adding magnesium chloride and sodium hydrogen phosphate solid, NH in ammonium chloride solution
4cl, MgCl
2, Na
2hPO
4molar ratio=2 ~ 4:1 ~ 2:1; Then the rapid NaOH solution of 1mol/L input in the solution system after adding magnesium chloride and sodium hydrogen phosphate is reacted, and is taken out by sediment dry.
3. application process according to claim 2, is characterized in that, the described synthetic method containing the crystalline hydrate mineral of amino and hydroxyl is specific as follows:
1) ammonium chloride solution of 2g/L is prepared in N, according to molar ratio n (NH
4cl): n (MgCl
2): n (Na
2hPO
4)=2 ~ 4:1 ~ 2:1 prepares quantitative magnesium chloride and sodium hydrogen phosphate solid, and prepares the NaOH solution of 1mol/L;
2) keeping under the condition stirred, in the ammonium chloride solution of preparation, adding magnesium chloride and sodium hydrogen phosphate solid, according to volume ratio v (NaOH): v (NH
4cl)=0.01 ~ 0.04:1, drops into the NaOH solution of 1mol/L rapidly in the solution system after adding magnesium chloride and sodium hydrogen phosphate; Maintenance system mixing speed is 400 ~ 600r/min, time 10 ~ 20min;
3) sediment is taken out drying, control baking temperature is 40-50 DEG C, time 2 ~ 6h.
4. the application process according to any one of claim 1-3, is characterized in that, specifically comprises the following steps during application:
(1) regulate zinc-containing water pH value, make to generate containing zinc hydroxide precipitation containing zinc ion generation hydrolysis;
(2) in the zinc hydroxide system after hydrolysis, add the crystalline hydrate mineral containing amino and hydroxyl;
(3) solid-liquid system of step (2) gained is carried out leave standstill, Separation of Solid and Liquid.
5. application process according to claim 4, is characterized in that, step (1) regulates zinc-containing water pH value to 6-7, and reaction time control is 10 ~ 20min.
6. application process according to claim 5, is characterized in that, step (1) uses the NaOH solution of 0.1mol/L or lime milk solution to regulate zinc-containing water pH value.
7. application process according to claim 4, is characterized in that, step (2) is 0.5 ~ 5.0:1.0 containing the mass ratio of zinc in the crystalline hydrate mineral dosage of amino and hydroxyl and system.
8. application process according to claim 4, is characterized in that, step (2) reaction time is 20 ~ 30min.
9. application process according to claim 4, is characterized in that, step (2) stir speed (S.S.) controls at 100 ~ 300r/min.
10. application process according to claim 4, is characterized in that, step (3) time of repose is 10 ~ 20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610066817.8A CN105521758B (en) | 2016-01-29 | 2016-01-29 | A kind of application method of crystalline hydrate mineral containing amino and hydroxyl in zinc-containing water processing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610066817.8A CN105521758B (en) | 2016-01-29 | 2016-01-29 | A kind of application method of crystalline hydrate mineral containing amino and hydroxyl in zinc-containing water processing |
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|---|---|
| CN105521758A true CN105521758A (en) | 2016-04-27 |
| CN105521758B CN105521758B (en) | 2019-03-05 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650587A (en) * | 1982-09-09 | 1987-03-17 | Akzona Incorporated | Ammonia scavenger |
| CN102211018A (en) * | 2011-06-16 | 2011-10-12 | 天津森诺过滤技术有限公司 | Membrane adsorbent for recycling nitrogen and phosphorus resources from waste water as well as preparation method and application thereof |
-
2016
- 2016-01-29 CN CN201610066817.8A patent/CN105521758B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650587A (en) * | 1982-09-09 | 1987-03-17 | Akzona Incorporated | Ammonia scavenger |
| CN102211018A (en) * | 2011-06-16 | 2011-10-12 | 天津森诺过滤技术有限公司 | Membrane adsorbent for recycling nitrogen and phosphorus resources from waste water as well as preparation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| ASHAKI A. ROUFF ET AL: ""Synergistic Removal of Zinc and Copper in Greenhouse Waste"", 《ACS SUSTAINABLE CHEMISTRY & ENGINEERING》 * |
| ASHAKI A. ROUFF ET AL: ""Zinc Interaction with Struvite During and After Mineral Formation"", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 * |
| ASHAKI A. S. A. LOBANOV ET AL: ""Treatment of Wastewater to Remove Ammonium Ions by Precipitation"", 《RUSSIAN JOURNAL OF APPLIED CHEMISTRY》 * |
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