CN106915811A - A kind of trivalent chromium passivation washings contact break agent and preparation method and application - Google Patents
A kind of trivalent chromium passivation washings contact break agent and preparation method and application Download PDFInfo
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- CN106915811A CN106915811A CN201511002549.5A CN201511002549A CN106915811A CN 106915811 A CN106915811 A CN 106915811A CN 201511002549 A CN201511002549 A CN 201511002549A CN 106915811 A CN106915811 A CN 106915811A
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- 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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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of trivalent chromium passivation washings contact break agent, it be with water-soluble metal salt as raw material, water as solvent, PAM as crosslinking agent, it is crosslinked obtained；Wherein, described water-soluble metal salt is two or more in water miscible zinc salt, ferrous salt, molysite, calcium salt or aluminium salt.The application of trivalent chromium passivation washings is being processed the invention also discloses trivalent chromium passivation washings contact break agent.The characteristics of trivalent chromium passivation washings contact break agent preparation process is simple of the present invention, effect is significant, extensive applicability；The crosslinking of contact break agent metal cation and PAM belongs to physical aspect, the presence of PAM can be such that metal cation is fully contacted with the complexing organic matter in waste water, promote interaction between the two, for processing the poaching wastewater of trivalent chromium passivation containing complex state, the trivalent chromium in complex state in waste water can effectively be removed, its potential threat to water environment is eliminated, the clearance of trivalent chromium can reach 99.9%.
Description
Technical field：
The invention belongs to electroplating wastewater innoxious process for treating field, and in particular to a kind of trivalent chromium passivation washings contact break agent and its
Preparation method and application.
Background technology：
For a long time, chromating has been widely used in plating and Surface Processing Industry, but Cr VI toxicity is big, is again to cause
Cancer material, severe contamination environment.Enhancing with people to environmental protection consciousness, the application of Cr VI is gradually strictly limited
System, therefore it is imperative to research and develop nontoxic or low toxicity material replacement chromating technique.At present, chromium-free deactivation and three
Valency chromium passivating has been achieved for positive progress, and trivalent chromium passivation has been widely used in production.But in order to obtain good passivation
Effect, must add substantial amounts of additive, conventional additive to include citric acid, tartaric acid, grape in trivalent chromium passivation plating solution
Saccharic acid, malic acid etc..The use of additive can be also complexed so as to increase while passivation quality is ensured with trivalent chromic ion
The stability of trivalent chromic ion, then causes the trivalent chromic ion in washings to be difficult to by traditional chemical precipitation method in strong plating solution
Removal, the crome metal of residual is not only potential pollution sources, can also increase the processing cost in later stage.
The chemical reaction process of traditional chemical precipitation method treatment trivalent chromium passivation washings is as follows：
10Cr3+-R+33OH-→Cr(OH)3↓+9Cr3+-R+30OH-
In formula：Cr3+- R refers to trivalent chromium complex ion, and R refers to additive.As can be seen that when addition from above-mentioned signal reaction equation
Enough OH-When only have a small amount of trivalent chromium to generate Cr (OH)3Precipitation, most of trivalent chromium is still in Cr3+- R complex states.
With the development of China's industrial level, the trivalent chromium passivation technique of low toxicity substitution Cr VI has been inevitable, but the technique is complete
Promote and still need to overcome in passivation washings that trivalent chromic ion stability is strong, be difficult to the problem of removal up to standard in face.
The content of the invention：
To solve above-mentioned problem, the present invention proposes a kind of trivalent chromium passivation washings contact break agent and preparation method thereof, contact break agent tool
The characteristics of having preparation process is simple, effect is significant, extensive applicability.
The purpose of the present invention is achieved through the following technical solutions：
A kind of trivalent chromium passivation washings contact break agent, it be with water-soluble metal salt as raw material, water as solvent, PAM (polypropylene
Acid amides) it is crosslinking agent, it is crosslinked obtained；Wherein, described water-soluble metal salt is water miscible zinc salt, ferrous salt, iron
Two or more in salt, calcium salt or aluminium salt.
Preferably, described trivalent chromium passivation washings contact break agent is as obtained in following preparation method：Weigh water-soluble metal salt
It is soluble in water to prepare the aqueous metal salt that substance withdrawl syndrome is 0.4~1.5mol/L, according to aqueous metal salt quality
5~15% are added in aqueous metal salt the PAM aqueous solution that mass percentage concentration is 2%, stir 10~20min best friends
Connection is complete, adjusts the pH of solution to 1~2, obtains trivalent chromium passivation washings contact break agent.
It is furthermore preferred that described trivalent chromium passivation washings contact break agent is as obtained in following preparation method：Weigh water-soluble metal
Salt is soluble in water to prepare the aqueous metal salt that substance withdrawl syndrome is 0.6~1.0mol/L, according to aqueous metal salt quality
6~7% are added in aqueous metal salt the PAM aqueous solution that mass percentage concentration is 2%, stir 10~20min best friends
Connection is complete, using mass fraction 10% sulfuric acid regulation solution pH to 1~2, obtain trivalent chromium passivation washings contact break agent.
Preferably, described water-soluble metal salt is ZnCl2、FeCl2、FeCl3、CaCl2、AlCl3In two or more.
Preferably, described water is deionized water.The running water without obvious impurity can also be used.
The present invention can also be using the hydrochloric acid or nitre acid for adjusting pH that can reach identical purpose.
The preparation method of trivalent chromium passivation washings contact break agent of the present invention, comprises the following steps：Weigh water-soluble metal salt
It is soluble in water to prepare the aqueous metal salt that substance withdrawl syndrome is 0.4~1.5mol/L, according to aqueous metal salt quality
5~15% are added in aqueous metal salt the PAM aqueous solution that mass percentage concentration is 2%, stir 10~20min best friends
Connection is complete, adjusts the pH of solution to 1~2, obtains trivalent chromium passivation washings contact break agent.
Preferably, described water is deionized water.The running water without obvious impurity can also be used.
Preferably, the slaine that water-soluble metal salt preparation substance withdrawl syndrome soluble in water is 0.6~1.0mol/L is weighed water-soluble
Liquid, metal salt solution is added to according to the 6~7% of aqueous metal salt quality by the PAM aqueous solution that mass percentage concentration is 2%
In solution, 10~20min of stirring is complete to being crosslinked, using mass fraction 10% sulfuric acid regulation solution pH to 1~2, obtain
To trivalent chromium passivation washings contact break agent.
Application of the trivalent chromium passivation washings contact break agent of the present invention in treatment trivalent chromium passivation washings.
Trivalent chromium passivation washings contact break agent of the present invention is used for the method for processing trivalent chromium passivation washings, including following step
Suddenly：
(1) pH value of regulation raw material trivalent chromium passivation washings is to 4~5；
(2) mixed liquor is obtained to addition contact break agent in trivalent chromium passivation washings；Control 300~400r/min of mixing speed,
5~15min of reaction time, makes above-mentioned mixed liquor fully react, and abolishes the complex status of trivalent chromium in waste water；
(3) pH value of reacted mixed liquor is adjusted to 10~11, controls 200~300r/min of mixing speed, reaction time
15~25min；Under the conditions of the pH, metal cation is fully contacted with the additive in waste water, promotes interaction；
(4) to the PAC (polyaluminiums that addition mass percentage concentration in the mixed liquor after being processed through step (3) is 10%
Aluminium) aqueous solution, maintain pH of mixed 10~11, control 200~300r/min of mixing speed, reaction time 5~15
min；The small suspended particulate of step reaction generation, reduces delivery turbidity before being flocculated by PAC；
(5) solution left standstill precipitation after reacting completely, supernatant is the water outlet after treatment.
In step (2), trivalent chromic ion in described trivalent chromium passivation washings contact break agent and raw material trivalent chromium passivation washings
Volume mass ratio be 1~2：10~20mL/mg, preferably 1~2.8：20mL/mg.
Using pH value in the NaOH reacted mixed liquors of regulation of mass fraction 30% to 10~11.
In step (4), trivalent chromic ion volume mass ratio is in the described PAC aqueous solution and raw material trivalent chromium passivation washings
1~2：50mL/mg, preferably 1~1.5：50mL/mg.
Reaction mechanism of the invention is analyzed as follows：
In trivalent chromium passivation poaching wastewater, Cr3+Exist in complex state form with additive R in water, such as Cr3+- R etc..
Cr3+-R+Mn+→Mn+-R+Cr3+
Cr3++OH-→Cr(OH)3↓
In formula：Mn+It is metal cation, can is Zn2+、Fe2+、Fe3+、Ca2+Or Al3+, R is citric acid, winestone
Acid, gluconic acid or malic acid.
Beneficial effects of the present invention：
The characteristics of trivalent chromium passivation washings contact break agent preparation process is simple of the present invention, effect is significant, extensive applicability.The present invention
The crosslinking of contact break agent metal cation and PAM belongs to physical aspect, and effect, the presence of PAM are not chemically bonded between the two
Metal cation can be made to be fully contacted with the complexing organic matter in waste water, promote interaction between the two, network is contained for processing
State trivalent chromium passivation poaching wastewater is closed, the trivalent chromium in complex state in waste water can be effectively removed, it is eliminated to the potential of water environment
Threaten, the clearance of trivalent chromium can reach 99.9%.
Specific embodiment：
Technical scheme is described further below by specific embodiment.
Embodiment 1
A kind of trivalent chromium passivation washings contact break agent, is obtained by following preparation method, is comprised the following steps：According to the amount of material
1：0.5：1：0.2 weighs water-soluble metal salt ZnCl2、FeCl2、CaCl2、AlCl3, with deionized water dissolving, it is configured to
Molar concentration is the aqueous metal salt of 0.6mol/L, is 2% by mass percentage concentration according to the 7% of aqueous metal salt quality
The PAM aqueous solution be added in aqueous metal salt, 10~20min of stirring is complete to being crosslinked, and the sulfuric acid for adding 10% is adjusted
Section pH obtains final product trivalent chromium passivation washings contact break agent to 1~2.
A kind of method that trivalent chromium passivation washings are processed using above-mentioned trivalent chromium passivation washings contact break agent, its step is as follows：
(1) raw material trivalent chromium passivation washings are in atropurpureus, and trivalent chromic ion concentration is 200mg/L；Regulation trivalent chromium passivation
Washings pH is 4~5；
(2) above-mentioned waste water 500mL is taken, trivalent chromium passivation washings contact break agent 5.0mL is added, mixed liquor is obtained；Control is stirred
Speed 300r/min is mixed, 10min is reacted, above-mentioned mixed liquor is fully reacted；
(3) to the NaOH that 30% is added in reacted mixed liquor, pH to 10.5 is adjusted, controls mixing speed 200
R/min, reaction time 15min；
(4) it is 10% PAC aqueous solution 2mL to addition mass percentage concentration in above-mentioned mixed liquor, and maintains pH of mixed
10.5, mixing speed 300r/min, reaction time 10min are controlled；
(5) staticly settled after reacting completely, supernatant water white transparency, water outlet trivalent chromic ion content is 0.16mg/L.
Embodiment 2
A kind of preparation method of trivalent chromium passivation washings contact break agent, comprises the following steps：According to molar concentration 1：0.8：0.5
Weigh soluble metallic salt ZnCl2、CaCl2、AlCl3, with deionized water dissolving, it is 1.0 to be configured to substance withdrawl syndrome
The aqueous metal salt of mol/L, according to aqueous metal salt quality 6% by the PAM aqueous solution that mass percentage concentration is 2%
Be added in aqueous metal salt, 10~20min of stirring is complete to being crosslinked, add 10% sulphur acid for adjusting pH to 1~
2, obtain final product trivalent chromium passivation washings contact break agent.
A kind of method that trivalent chromium passivation washings are processed using above-mentioned trivalent chromium passivation washings contact break agent, its step is as follows：
(1) raw material trivalent chromium passivation washings trivalent chromic ion concentration 100mg/L, waste water is in atropurpureus, adjusts wastewater pH
It is 4~5；
(2) above-mentioned waste water 500mL is taken, trivalent chromium passivation washings contact break agent 7mL is added, mixing speed 300 is controlled
R/min, reacts 10min；
(3) 30% NaOH is added, pH to 11 is adjusted, mixing speed 250r/min, reaction time 20min is controlled；
(4) to the PAC aqueous solution 1.5mL of addition 10% in above-mentioned mixed liquor, and pH of mixed to 10.5 is maintained, is controlled
Mixing speed 200r/min, reaction time 5min；
(5) staticly settled after reacting completely, supernatant water white transparency, water outlet trivalent chromium content is 0.08mg/L.
Comparative example
The technique that trivalent chromium passivation washings are processed using the traditional chemical precipitation method, its step is as follows：
(1) raw material trivalent chromium passivation washings are in atropurpureus, and trivalent chromic ion content is 200mg/L；
(2) above-mentioned waste water 500mL is taken, 30% NaOH is added, pH to 10.5 is adjusted, mixing speed 200 is controlled
R/min, reaction time 15min；
(4) it is 10% PAC solution 2mL to addition mass percentage concentration in above-mentioned mixed liquor, and maintains pH of mixed to exist
10.5, control mixing speed 300r/min, reaction time 10min；
(5) staticly settled after reacting completely, supernatant is still in atropurpureus, water outlet trivalent chromic ion content is 162.3mg/L.
Claims (10)
1. a kind of trivalent chromium passivation washings contact break agent, it is characterised in that the contact break agent be with water-soluble metal salt as raw material, water
It is crosslinked obtained for solvent, PAM are crosslinking agent；Wherein, described water-soluble metal salt is water miscible zinc salt, Asia
Two or more in molysite, molysite, calcium salt or aluminium salt.
2. trivalent chromium passivation washings contact break agent according to claim 1, it is characterised in that described trivalent chromium passivation drift
Wash water contact break agent is as obtained in following preparation method：Weighing water-soluble metal salt substance withdrawl syndrome of preparing soluble in water is
The aqueous metal salt of 0.4~1.5mol/L, is 2% by mass percentage concentration according to the 5~15% of aqueous metal salt quality
The PAM aqueous solution is added in aqueous metal salt, and 10~20min of stirring is complete to being crosslinked, adjust the pH to 1 of solution~
2, obtain trivalent chromium passivation washings contact break agent.
3. trivalent chromium passivation washings contact break agent according to claim 2, it is characterised in that described trivalent chromium passivation drift
Wash water contact break agent is as obtained in following preparation method：Weighing water-soluble metal salt substance withdrawl syndrome of preparing soluble in water is
The aqueous metal salt of 0.6~1.0mol/L, is 2% by mass percentage concentration according to the 6~7% of aqueous metal salt quality
The PAM aqueous solution is added in aqueous metal salt, and 10~20min of stirring is complete to being crosslinked, using the sulphur of mass fraction 10%
The pH of acid-conditioning solution obtains trivalent chromium passivation washings contact break agent to 1~2.
4. the trivalent chromium passivation washings contact break agent according to claim 1,2 or 3, it is characterised in that described water solubility
Slaine is ZnCl2、FeCl2、FeCl3、CaCl2、AlCl3In two or more；Described water is deionized water.
5. the preparation method of the trivalent chromium passivation washings contact break agent described in claim 1, it is characterised in that including following step
Suddenly：The aqueous metal salt that water-soluble metal salt preparation substance withdrawl syndrome soluble in water is 0.4~1.5mol/L is weighed, according to
The PAM aqueous solution that mass percentage concentration is 2% is added to aqueous metal salt by the 5~15% of aqueous metal salt quality
In, 10~20min of stirring is complete to being crosslinked, and adjusts the pH of solution to 1~2, obtains trivalent chromium passivation washings contact break agent.
6. the preparation method of trivalent chromium passivation washings contact break agent according to claim 5, it is characterised in that including as follows
Step：The aqueous metal salt that water-soluble metal salt preparation substance withdrawl syndrome soluble in water is 0.6~1.0mol/L is weighed, is pressed
The PAM aqueous solution that mass percentage concentration is 2% is added to aqueous metal salt by according to aqueous metal salt quality 6~7%
In, 10~20min of stirring is complete to being crosslinked, using mass fraction 10% sulfuric acid regulation solution pH to 1~2, obtain three
Valency chromium passivating washings contact break agent.
7. the preparation method of the trivalent chromium passivation washings contact break agent according to claim 5 or 6, it is characterised in that described
Water-soluble metal salt be ZnCl2、FeCl2、FeCl3、CaCl2、AlCl3In two or more；Described water is deionization
Water.
8. the trivalent chromium passivation washings contact break agent described in claim 1,2,3 or 4 is in treatment trivalent chromium passivation washings
Using.
9. the trivalent chromium passivation washings contact break agent described in claim 1 is used for the method for processing trivalent chromium passivation washings, its
It is characterised by comprising the following steps：
(1) pH value of regulation raw material trivalent chromium passivation washings is to 4~5；
(2) mixed liquor is obtained to addition contact break agent in trivalent chromium passivation washings；Control 300~400r/min of mixing speed,
5~15min of reaction time, makes above-mentioned mixed liquor fully react；
(3) pH value of reacted mixed liquor is adjusted to 10~11, controls 200~300r/min of mixing speed, reaction time
15~25min；
(4) to the PAC aqueous solution that mass percentage concentration is 10% is added in the mixed liquor after being processed through step (3), maintain
PH of mixed controls 200~300r/min of mixing speed, 5~15min of reaction time 10~11；
(5) solution left standstill precipitation after reacting completely, supernatant is the water outlet after treatment.
10. trivalent chromium passivation washings contact break agent according to claim 9 is used to process the side of trivalent chromium passivation washings
Method, it is characterised in that in step (2), in described trivalent chromium passivation washings contact break agent and raw material trivalent chromium passivation washings
The volume mass ratio of trivalent chromic ion is 1~2：10~20mL/mg, preferably 1~2.8：20mL/mg；
In step (4), trivalent chromic ion volume mass ratio is in the described PAC aqueous solution and raw material trivalent chromium passivation washings
1~2：50mL/mg, preferably 1~1.5：50mL/mg.
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| CN110642425A (en) * | 2019-10-12 | 2020-01-03 | 广州超邦化工有限公司 | Treatment method of trivalent chromium passivation wastewater containing hydrofluoric acid and carboxylic acid |
| CN110642395A (en) * | 2019-10-12 | 2020-01-03 | 广州超邦化工有限公司 | Method for treating fluoride ion-containing sulfate trivalent chromium plating wastewater |
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| CN110759512A (en) * | 2018-07-27 | 2020-02-07 | 广州超邦化工有限公司 | Novel method for treating potassium chloride cyanide-free cadmium plating wastewater |
| CN110790418A (en) * | 2018-08-02 | 2020-02-14 | 广州超邦化工有限公司 | Treatment method of potassium chloride cyanide-free cadmium plating and passivation mixed wastewater |
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| CN110790417B (en) * | 2018-08-02 | 2021-12-24 | 广州超邦化工有限公司 | Treatment method of hardware and electronic electroplating wastewater |
| CN110790416B (en) * | 2018-08-02 | 2021-11-19 | 广州超邦化工有限公司 | Method for treating electroless copper plating wastewater |
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| CN110818123B (en) * | 2018-08-10 | 2021-11-19 | 广州超邦化工有限公司 | Treatment method of trivalent chromium plating waste water |
| CN110818123A (en) * | 2018-08-10 | 2020-02-21 | 广州超邦化工有限公司 | Treatment method of trivalent chromium plating waste water |
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| CN110642425A (en) * | 2019-10-12 | 2020-01-03 | 广州超邦化工有限公司 | Treatment method of trivalent chromium passivation wastewater containing hydrofluoric acid and carboxylic acid |
| CN110642395A (en) * | 2019-10-12 | 2020-01-03 | 广州超邦化工有限公司 | Method for treating fluoride ion-containing sulfate trivalent chromium plating wastewater |
| CN110642425B (en) * | 2019-10-12 | 2021-10-08 | 广州超邦化工有限公司 | Treatment method of trivalent chromium passivation wastewater containing hydrofluoric acid and carboxylic acid |
| CN113860458A (en) * | 2021-10-09 | 2021-12-31 | 郑州大学 | Composite chelating agent and preparation method and application thereof |
| CN113860458B (en) * | 2021-10-09 | 2023-09-12 | 郑州大学 | Composite chelating agent and preparation method and application thereof |
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