CN108083509B - Adsorption column type stainless steel pickling waste liquid treatment and recovery method - Google Patents
Adsorption column type stainless steel pickling waste liquid treatment and recovery method Download PDFInfo
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- 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
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
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- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C02F2303/16—Regeneration of sorbents, filters
Abstract
The invention relates to an adsorption column type stainless steel pickling waste liquid treatment and recovery method, which sequentially comprises the following steps of (1) adsorbing chromium: passing the acid pickling waste liquid through an adsorption column A at the flow rate of 0.5-0.8ml/min, filling ceramic particles A in the adsorption column A, filling 15-20g of ceramic particles A in each 100mg/l of chromium ions, and carrying out alkali washing desorption on the adsorption column A to recover chromium; (2) precipitating iron: the liquid flowing out of the adsorption column A enters a treatment tank, and the pH value is adjusted to generate ferric hydroxide; (3) and (3) nickel adsorption: the liquid flowing out of the treatment tank sequentially enters an adsorption column B and an adsorption column C filled with ceramic particles B at the flow rate of 0.5-0.8ml/min, the ceramic particles B are formed by burning phosphate rock powder, bentonite and bamboo powder, and nickel is recovered by alkali washing, desorption and adsorption column C; the liquid passing through the adsorption column C is acid liquor for removing chromium, iron and nickel ions. The invention establishes a method for treating and recycling the pickling waste liquid, which has low treatment cost and can efficiently recycle iron, chromium and nickel ions.
Description
Technical Field
The invention relates to a process method for treating heavy metal wastewater, which is mainly suitable for treating and recycling waste acid generated in stainless steel production and heavy metal in wastewater generated in similar industries.
Background
Toxic metal ions are harmful to human bodies, heavy metals such as chromium, iron, selenium, vanadium, copper, cobalt, nickel, cadmium, mercury, silver, lead, zinc and the like have special toxicity, and after industrial and other domestic wastewater containing the heavy metals is discharged, the generated heavy metals can form lasting and accumulative characteristics in nature. The existence of many metal ions, especially toxic heavy metals, in industrial wastewater has become an important environmental problem, and the influence of heavy metals on the human ecosystem has received more and more attention. Wastewater discharged from many industries (mining, stainless steel, chemical, metallurgical, and battery) contains heavy metals such as chromium, cadmium, iron, nickel, and lead, among which cr (iv) has a relatively high toxicity even at low concentrations.
Conventional methods for removing metal ions from aqueous solutions include chemical precipitation, chemical oxidation/reduction, reverse osmosis, electrodialysis, ultrafiltration, and the like. However, these conventional techniques have their own inherent limitations, such as low efficiency, high production cost, complicated operating conditions, difficulty in further treatment of secondary sludge, waste of resources, and the like. The adsorption technology is used for removing heavy metals, is simple to operate, is not influenced by the toxicity of target pollutants, and does not need dangerous chemicals. In addition, if desired, adsorption facilitates concentration, and the adsorbed material can then be recycled.
At present, some new process methods and recovery methods for wastewater treatment are developed, but some processes cannot be completely applied to the characteristics that waste acid generated in stainless steel production has large iron and nickel ion content and other wastewater metal ions have large fluctuation. The adsorption technology is combined with a simple chemical treatment process, so that the novel process design and application for achieving the purposes of simple operation, low cost and wastewater recycling and metal recovery have important significance for treating wastewater generated by production, particularly have obvious social and economic benefits for recycling waste acid and metal in stainless steel pickling production wastewater, and have reference and promotion effects on similar wastewater treatment in other industries. The novel wastewater treatment process has the advantages of secondary utilization of resources, simple process, high treatment efficiency, cyclic utilization of wastewater, realization of zero discharge of wastewater or discharge of a small amount of wastewater reaching the standard, bidirectional benefits on production and environment, and important development trend of water treatment in future.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for treating and recovering the adsorption column type stainless steel pickling waste liquid, which realizes the aim of efficiently recovering iron, chromium and nickel ions while ensuring low cost.
The scheme for solving the technical problems comprises the following steps:
the method for treating and recovering the adsorption column type stainless steel pickling waste liquid sequentially comprises the following steps,
(1) adsorbing chromium: the pickling waste liquid passes through an adsorption column A, ceramic particles A are filled in the adsorption column A, the ceramic particles A are formed by firing bamboo powder and bentonite, the using amount of the ceramic particles A is adjusted according to the content of chromium ions in the original pickling waste liquid, and 15-20g of the ceramic particles A are filled in each 100mg/l of chromium ions; the flow rate of the pickling waste liquid in the adsorption column A is 0.5-0.8 ml/min; after the acid pickling waste liquid flows out of the adsorption column A, carrying out alkali washing desorption on the adsorption column A, and recovering chromium from the desorption liquid;
(2) precipitating iron: the liquid flowing out of the adsorption column A enters a treatment tank, the pH value of the liquid entering the treatment tank is adjusted to 4-6 by using alkaline water to generate ferric hydroxide, and the ferric hydroxide in the treatment tank is recovered after the liquid is filtered;
(3) and (3) nickel adsorption: liquid flowing out of the treatment tank sequentially enters an adsorption column B and an adsorption column C, ceramic particles B are filled in the adsorption column B and the adsorption column C, the ceramic particles B are formed by burning phosphate rock powder, bentonite and bamboo powder, the dosage of the ceramic particles B is adjusted according to the content of nickel ions in the original pickling waste liquid, and 80-100g of the ceramic particles B are filled in the adsorption column B and the adsorption column C respectively every 100mg/l of the nickel ions; the flow rates of the pickling waste liquid in the adsorption column B and the adsorption column C are both 0.5-0.8 ml/min; after the pickling waste liquid flows out of the adsorption column B and the adsorption column C, carrying out alkali washing desorption on the adsorption column B and the adsorption column C, and recovering nickel from the desorption liquid; the liquid passing through the adsorption column C is acid liquor for removing chromium, iron and nickel ions.
As an improvement, the mass ratio of the bamboo powder to the bentonite in the ceramic particles A is 50-70: 50-30.
As a refinement, the particle size of the ceramic particles A is 4-6 mm.
As an improvement, P in the ground phosphate rock2O5The content of (B) is 5-10 mass%.
As a further improvement, the mass ratio of the phosphorus mineral powder, the bentonite and the bamboo powder in the ceramic particles B is 50-70: 40-20: 10.
As a refinement, the particle size of the ceramic particles B is 4-6 mm.
As a further improvement, the acid solution after passing through the adsorption column C is reused as acid for acid washing in the original production after supplementing the reduced acid amount in the step (2).
As a further improvement, in the steps (1) and (3), the alkaline water after the alkali elution is used as the alkaline water for adjusting the pH in the step (2).
As a further improvement, the number of the adsorption columns A is 2, 2 adsorption columns A alternately operate, wherein when 1 adsorption column A performs adsorption operation, the other adsorption column A performs alkali washing desorption; the number of the adsorption columns B and the number of the adsorption columns C are 2, the adsorption columns B and the adsorption columns C are alternately operated, and when 1 adsorption column B and 1 adsorption column C are subjected to adsorption operation, the other adsorption column B and the other adsorption column C are subjected to alkali washing desorption.
The ceramic particles of the present invention are relatively inexpensive to manufacture, but have very strong adsorption capacity for chromium and nickel. The method not only has less reagent consumption, but also realizes the high-efficiency recovery of iron, chromium and nickel metal oxide resources, realizes the recycling of mixed acid of the ortho-acid washing nitric acid and the hydrofluoric acid, recycles the elution attached wastewater and has obvious economic benefit. More importantly, after the method is adopted, the waste water discharge is less, the zero discharge can be almost realized, and the social benefit is remarkable.
Drawings
FIG. 1 is a process diagram of the present invention, wherein the solid lines represent the adsorption of chromium and nickel ions and the precipitation of iron ions and the circulation route of acid solution, and the dotted lines represent the desorption of chromium and nickel ions and the flow route of alkali solution.
Detailed Description
The invention is further illustrated by the following specific procedures and examples.
As shown in FIG. 1, the operation process flow of the invention is as follows: 2 sets of adsorption columns are adopted, the number of the adsorption columns A, the number of the adsorption columns B and the number of the adsorption columns C are 2, the 2 sets of adsorption columns can alternately operate, and when 1 adsorption column A performs adsorption operation, the other adsorption column A can perform alkali washing desorption; when 1 of the adsorption columns B and 1 of the adsorption columns C are used for adsorption operation, the other adsorption column B and the other adsorption column C can be subjected to alkali washing desorption. The operation process has the characteristics of simple structure, high adsorption rate, good independent and separate recovery effect, low operation cost, no waste liquid discharge and high production efficiency.
Example 1
100ml of pickling waste liquid (containing 439.6mg/l, 79010.8mg/l and 18486.8mg/l of chromium, iron and nickel respectively) is taken and sequentially treated by the following steps:
(1) adsorbing chromium: and (3) passing the pickling waste liquid through an adsorption column A, wherein ceramic particles A are filled in the adsorption column A.
The ceramic particles a are characterized in that: a. the ceramic particles A are formed by firing bamboo powder and bentonite, and the mass ratio of the bamboo powder to the bentonite is 50-70: 50-30; b. the grain diameter of the ceramic grains A is 4-6 mm; c. the preparation process of the ceramic particles A can be created by referring to the invention with the application number of 201610922374.8.
Adjusting the dosage of the ceramic particles A according to the content of chromium ions in the original pickling waste liquid, wherein 15-20g of the ceramic particles A are filled in each 100mg/l of chromium ions, and the dosage standard of the ceramic particles A in the embodiment is that 20g of the ceramic particles A are filled in each 100mg/l of chromium ions; the flow rate of the waste pickle liquor in the adsorption column A is 0.5-0.8 ml/min.
After the acid pickling waste liquid flows out of the adsorption column A, carrying out alkali washing desorption on the adsorption column A, and recovering chromium from the desorption liquid;
(2) precipitating iron: and (3) enabling the liquid flowing out of the adsorption column A to enter a treatment tank, adjusting the pH value of the liquid entering the treatment tank to be 4-6, in the embodiment, adjusting the pH value to be 5-6 to generate ferric hydroxide, and recovering the ferric hydroxide in the treatment tank after filtering the liquid.
(3) And (3) nickel adsorption: and liquid flowing out of the treatment tank sequentially enters an adsorption column B and an adsorption column C, and ceramic particles B are filled in the adsorption column B and the adsorption column C.
The ceramic particles B are characterized in that: a. the ceramic particles B are formed by firing phosphate rock powder, bentonite and bamboo powder, and the mass ratio of the phosphate rock powder, the bentonite and the bamboo powder in the ceramic particles B is 50-70: 40-20: 10; b. the grain diameter of the ceramic grains B is 4-6 mm; c. the preparation process of the ceramic particles B can be created by referring to the invention with the application number of 201610922374.8, and can also be prepared by the following method: mixing ground phosphate rock (containing P)2O55-10 percent of bentonite and bamboo powder are mixed according to a certain proportion to prepare balls, and after drying, the balls are covered with diatomiteThe temperature is raised at the speed of 5 ℃/min, when the temperature is raised to 1000 ℃, the temperature is kept for 1 hour, and the furnace is cooled to the room temperature.
Adjusting the dosage of the ceramic particles B according to the content of nickel ions in the original pickling waste liquid, wherein 80-100g of nickel ions are respectively filled in the adsorption column B and the adsorption column C per 100mg/l of nickel ions, and 100g of nickel ions are filled in the embodiment; the flow rates of the pickling waste liquid in the adsorption column B and the adsorption column C are both 0.5-0.8 ml/min;
after the pickling waste liquid flows out of the adsorption column B and the adsorption column C, carrying out alkali washing desorption on the adsorption column B and the adsorption column C, and recovering nickel from the desorption liquid; the liquid passing through the adsorption column C is acid liquor for removing chromium, iron and nickel ions.
The acid solution after passing through the adsorption column C can be reused in the original production as acid for acid washing after supplementing the acid amount reduced in the step (2). In the steps (1) and (3), the alkaline water after the alkali elution can be used as the alkaline water for adjusting the pH in the step (2).
After the treatment of the steps, the result of the atomic absorption measurement of the clear liquid is as follows: the adsorption rates of chromium, iron and nickel were found to be 98.5%, 99.9% and 95.2%, respectively. And (3) obtaining a clear solution which is the mixed acid of nitric acid and hydrofluoric acid for removing heavy metal ions, and supplementing the acid amount (supplementing the mixed acid of nitric acid and hydrofluoric acid) reduced when the pH is adjusted in the treatment process according to the requirement of the mixed acid required by actual production, wherein the pH is adjusted to be about 0.5 and is recycled to the acid for the acid pickling process.
And (3) desorbing the adsorption column by using alkali, using 0.1mol/l of desorption reagent and 50ml of NaOH, oscillating for 6h, reducing the pH of desorption solution to about 13, recovering chromium hydroxide from the filtrate after the chromium-containing desorption column is washed, and recovering nickel hydroxide from the filtrate after the nickel-containing desorption column is washed. And (5) recycling clear liquid, and using the clear liquid as alkaline water for adjusting the pH value of the filter tank.
Example 2
Compared with the embodiment 1, the embodiment 2 has different parameters, specifically: the using amount of the ceramic particles A in the step (1) is 15g, and the oscillation time is 6 hours; adjusting the pH value to 4-5 in the step (2); in the step (3), the loading amount of the ceramic particles B in the adsorption column B and the adsorption column C is 80 g. After treatment, the results of the atomic absorption measurements of the clear liquid are: the adsorption rates of chromium, iron and nickel were 97.6%, 99.8% and 93.5%, respectively.
Claims (9)
1. The method for treating and recovering the adsorption column type stainless steel pickling waste liquid is characterized by comprising the following steps: the method sequentially comprises the following steps of,
(1) adsorbing chromium: the pickling waste liquid passes through an adsorption column A, ceramic particles A are filled in the adsorption column A, the ceramic particles A are formed by firing bamboo powder and bentonite, the using amount of the ceramic particles A is adjusted according to the content of chromium ions in the original pickling waste liquid, and 15-20g of the ceramic particles A are filled in each 100mg/l of chromium ions; the flow rate of the pickling waste liquid in the adsorption column A is 0.5-0.8 ml/min; after the acid pickling waste liquid flows out of the adsorption column A, carrying out alkali washing desorption on the adsorption column A, and recovering chromium from the desorption liquid;
(2) precipitating iron: the liquid flowing out of the adsorption column A enters a treatment tank, the pH value of the liquid entering the treatment tank is adjusted to 4-6 by using alkaline water to generate ferric hydroxide, and the ferric hydroxide in the treatment tank is recovered after the liquid is filtered;
(3) and (3) nickel adsorption: liquid flowing out of the treatment tank sequentially enters an adsorption column B and an adsorption column C, ceramic particles B are filled in the adsorption column B and the adsorption column C, the ceramic particles B are formed by burning phosphate rock powder, bentonite and bamboo powder, the dosage of the ceramic particles B is adjusted according to the content of nickel ions in the original pickling waste liquid, and 80-100g of the ceramic particles B are filled in the adsorption column B and the adsorption column C respectively every 100mg/l of the nickel ions; the flow rates of the pickling waste liquid in the adsorption column B and the adsorption column C are both 0.5-0.8 ml/min; after the pickling waste liquid flows out of the adsorption column B and the adsorption column C, carrying out alkali washing desorption on the adsorption column B and the adsorption column C, and recovering nickel from the desorption liquid; the liquid passing through the adsorption column C is acid liquor for removing chromium, iron and nickel ions.
2. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: the mass ratio of the bamboo powder to the bentonite in the ceramic particles A is 50-70: 50-30.
3. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: the grain diameter of the ceramic grains A is 4-6 mm.
4. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: p in the ground phosphate rock2O5The content of (B) is 5-10 mass%.
5. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: the mass ratio of the phosphorus mineral powder, the bentonite and the bamboo powder in the ceramic particles B is 50-70: 40-20: 10.
6. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: the grain diameter of the ceramic grains B is 4-6 mm.
7. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: and (3) supplementing the acid amount reduced in the step (2) with the acid solution passing through the adsorption column C, and recycling the acid solution as acid for acid washing to the original production.
8. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: in the steps (1) and (3), the alkaline water after the alkali elution is used as the alkaline water for adjusting the pH in the step (2).
9. The method for treating and recovering the stainless steel pickling waste liquid of claim 1, which comprises the steps of: the number of the adsorption columns A is 2, 2 adsorption columns A alternately operate, wherein when 1 adsorption column A performs adsorption operation, the other adsorption column A performs alkali washing desorption; the number of the adsorption columns B and the number of the adsorption columns C are 2, the adsorption columns B and the adsorption columns C are alternately operated, and when 1 adsorption column B and 1 adsorption column C are subjected to adsorption operation, the other adsorption column B and the other adsorption column C are subjected to alkali washing desorption.
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| CN101982433A (en) * | 2010-11-09 | 2011-03-02 | 南京大学 | Method for harmless and recycling treatment of stainless steel acid washing waste water neutralization sludge |
| CN106378115A (en) * | 2016-06-15 | 2017-02-08 | 浙江工业大学 | Hierarchical-porous-structure bamboo charcoal/bentonite composite material and application thereof |
| CN106478069A (en) * | 2016-10-14 | 2017-03-08 | 湖州师范学院 | Bamboo charcoal bentonite composite ceramic material and preparation method thereof |
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Application publication date: 20180529 Assignee: Zhejiang Guanying Auto Parts Co.,Ltd. Assignor: HUZHOU TEACHERS College Contract record no.: X2023990000126 Denomination of invention: Treatment and recovery method of stainless steel pickling waste liquid with adsorption column Granted publication date: 20200825 License type: Exclusive License Record date: 20230112 |