CN105884082A - Method for treating acid wastewater in titanium dioxide production process through chlorination method - Google Patents
Method for treating acid wastewater in titanium dioxide production process through chlorination method Download PDFInfo
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- CN105884082A CN105884082A CN201610364216.5A CN201610364216A CN105884082A CN 105884082 A CN105884082 A CN 105884082A CN 201610364216 A CN201610364216 A CN 201610364216A CN 105884082 A CN105884082 A CN 105884082A
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- Prior art keywords
- carbide slag
- titanium dioxide
- waste water
- production process
- acid waste
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- 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
-
- 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
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Abstract
The invention relates to a wastewater treatment method and provides a method for treating acid wastewater in the titanium dioxide production process through a chlorination method. Carbide slag raw slurry is pumped from a carbide slag slurry pond in the acetylene generation procedure of a factory of polyvinyl chloride produced through a calcium carbide method, and carbide slag slurry is obtained after coarse solid insoluble substances are separated out through a cyclone hydraulic separator and is conveyed to a carbide slag slurry storage tank; the carbide slag slurry is added into a neutralization pond through a conveying pump and has neutralization reaction with acid wastewater; the mixture obtained after the reaction flows into a waste liquid settling pond to be settled, precipitate thick slurry flows into a thick slurry storage tank and is then conveyed to a filter press through a thick slurry conveying pump for filter pressing, and filter cakes are formed after washing. According to the method, the treatment process is short, operation is easy, production and operation management is convenient, waste is used for waste treatment in the whole treatment process, and cost for purchasing, stacking and slurrying of lime powder in the acid wastewater treatment process is reduced; in the whole treatment process, liquid is conveyed in a sealed mode, and the site environment is clean and hygienic; the filter cakes are used as raw materials of cement production, achieve comprehensive utilization of titanium dioxide slag and are economical and environmentally friendly.
Description
Technical field
The present invention relates to a kind of method of wastewater treatment, waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process
Processing method.
Background technology
Titanium dioxide is a kind of white inorganic pigment, has optimal opacity, optimal whiteness and brightness and nothing
The characteristics such as poison, being recognized is the Chinese white that at present performance is best in the world, be widely used in coating, plastics,
The industry such as papermaking, printing-ink, chemical fibre, rubber, cosmetics.
After richness titanium material is mainly mixed by chloridising production titanium dioxide with petroleum coke, chlorination furnace carries out chlorination
Reduction reaction, generates the mixture containing titanium tetrachloride, from chlorination furnace top mixture out through cyclone dust removal
Device separation slag, dirt, obtain crude titanic chloride；Make contained VOCl in crude titanic chloride3In impurity and mineral oil etc.
Reaction is except vanadium, and obtains refined titanic chloride after rectification；Refined titanic chloride at high temperature generates dioxy with oxygen reaction
Change titanio material, then obtain the Rutile type titanium dioxide of top grade through post processing.The dominant response principle of this technique is such as
Under:
Chlorination reaction 2TiO2+3C+4Cl2→2TiCl4+CO2+2CO
Oxidation reaction TiCl4+O2→TiO2+2Cl2
In chlorination reaction process, cyclone separator top expellant gas enters three grades of condenser condensations, from three
Level condenser overhead and rectifying column top out containing CO, CO2, HCl, unreacted Cl2TiCl with trace4
Deng chlorinated exhaust send chlorinated exhaust processing system to process.At present to chlorinated exhaust generally by pickling, alkali cleaning
Process, first pass through pickling and remove the wherein sour gas such as HCl and generate waste hydrochloric acid, then passing through alkali
Wash chlorine in process waste gas.The waste hydrochloric acid generated can not directly use due to impurity content height or sell, and is usually
Enter Waste Water Treatment, return chlorination slurrying by supplementing water as slurrying after neutralizing, precipitate, filtering.From
The impurity coke of discharge, FeCl bottom cyclone separator3、MgCl2、CaCl2, the complete titanium ore of unreacted etc. enters
In slurrying groove, using waste hydrochloric acid to carry out slurrying, the mixed liquor after gained slurrying is miscellaneous by solid with being pumped into pressure filter
Matter filter pressing, can return to after drying in chlorination furnace again as raw material reaction.Filtrate alkaline absorbent after filter pressing
The alkaline matter neutralisation treatment such as lime cream serosity or sodium hydroxide.
In Titanium Dioxide Produced by Chloride Procedure production process acid waste water include waste hydrochloric acid that pickling chlorinated exhaust obtains and
Filtrate after filter pressing, the process to acid waste water at present mainly purchases pulverized limestone as alkali liquor absorption agent so that
There is the stacking of pulverized limestone in Titanium Dioxide Produced by Chloride Procedure production scene, causes dust pollution, affects environment, and increases
The processing cost of enterprise；Hydroxide filtering residue after neutralization does not the most comprehensively utilize, and hydroxide filtering residue is stacked
Too increase stacking cost and the environmental effect of enterprise.
The acetylene generation operation of generated by polyvinyl chloride by calcium carbide device will produce substantial amounts of carbide slag slurries, polrvinyl chloride per ton
Product about by-product 7.7m3Carbide slag slurries, Ca (OH) in slurry2Mass content is based on 20%.According to " chlor-alkali (burns
Alkali, polrvinyl chloride) industry access condition " in regulation " newly-built, reorganization and expansion generated by polyvinyl chloride by calcium carbide project is necessary
The carbide slag comprehensive utilization device such as auxiliary construction carbide slag controlling the water circulation mud simultaneously ".
Summary of the invention
The technical problem to be solved is to provide acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process
Processing method, it is possible to utilize carbide slag slurries replace outsourcing pulverized limestone, in Titanium Dioxide Produced by Chloride Procedure production process acid
Property waste water is neutralized process, the treatment of wastes with processes of wastes against one another.
The technical solution adopted for the present invention to solve the technical problems is: acid in Titanium Dioxide Produced by Chloride Procedure production process
The processing method of waste water, comprises the following steps:
(1) carbide slag oleo stock is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation,
After thick solid insoluble isolated by cyclone hydraulic separators, obtain carbide slag slurries deliver to carbide slag slurries storage tank；
(2) carbide slag slurries in carbide slag slurries storage tank is in delivery pump joins neutralization pond and acid waste water is carried out
And reaction；
(3) step (2) neutralize reacted mixture flow into waste liquid sedimentation tank precipitate, precipitate underflow
Liquid is from flowing into underflow liquid storage tank, then is delivered to form filter cake after pressure filter carries out filter pressing, washing by dense slurry feeding pump；
In waste liquid sedimentation tank, supernatant is sent to clean solution tank.
Further, in described step (2), the mass flow ratio of acid waste water and carbide slag slurries is 1.3-1.7.
Further, in described step (1) the isolated thick solid insoluble particle diameter of cyclone hydraulic separators at 40 mesh
Below.
Further, in described step (3), the supernatant in clean solution tank is back to slurrying groove to cyclone separator
The impurity that bottom is discharged carries out slurrying or is used as the cleaning mixture of chlorinated exhaust.
Further, step (3) described pressure filter is diaphragm filter press.
Further, precipitate underflow liquid is after diaphragm filter press filters, then water flowing washing, removes solubility thing
Matter, then diaphragm filter press is pressurized to 5.5-6.5bar, from filter cake, extrude moisture content, the most again with compression sky
Free water in filter cake is blown out to obtain hydroxide filter cake by gas.
Further, described hydroxide filter cake is used as to produce the raw material of cement.
The invention has the beneficial effects as follows: the present invention uses carbide slag slurries to process in Titanium Dioxide Produced by Chloride Procedure production process
Acid waste water, handling process is short, simple to operate, be easy to normal operation, it is achieved that the treatment of wastes with processes of wastes against one another；Save
The expense such as the buying of pulverized limestone, stacking, slurrying in acid waste water processing procedure；Whole processing procedure is liquid
Body closes conveying, site environment sanitation and hygiene；After neutralizing reaction, filter cake is used as the raw material of manufacture of cement, it is achieved that
The comprehensive utilization of titanium dioxide waste residue, economic and environment-friendly.It is simultaneously achieved titanium dioxide industry and generated by polyvinyl chloride by calcium carbide
Industry, the highlights correlations of carbide slag cement industry.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
As it is shown in figure 1, the processing method of acid waste water in the present invention a kind of Titanium Dioxide Produced by Chloride Procedure production process, bag
Include following steps:
(1) carbide slag oleo stock is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation,
After thick solid insoluble isolated by cyclone hydraulic separators, obtain carbide slag slurries deliver to carbide slag slurries storage tank；
(2) carbide slag slurries in carbide slag slurries storage tank joins neutralization pond and acid waste water after delivery pump measures
It is neutralized reaction；
(3) step (2) neutralize reacted mixture flow into waste liquid sedimentation tank precipitate, precipitate underflow
Liquid is from flowing into underflow liquid storage tank, then is delivered to form filter cake after pressure filter carries out filter pressing, washing by dense slurry feeding pump；
In waste liquid sedimentation tank, supernatant is sent to clean solution tank.
In the present invention, its Main Ingredients and Appearance of carbide slag slurries is Ca (OH)2, and Ca (OH)2Content is 18～20%；Chlorination
Acid waste water in method production process of titanium pigment includes waste hydrochloric acid that pickling chlorinated exhaust obtains and divides from whirlwind
The impurity coke of discharge, FeCl bottom device3、MgCl2、CaCl2, the complete titanium ore of unreacted etc. enter slurrying groove
In, use waste hydrochloric acid to carry out slurrying, the mixed liquor after slurrying is with being pumped into pressure filter by solid impurity filter pressing, pressure
Filtrate after filter；And acid waste water major part is from the filtrate after slurrying filter pressing.
In neutralization pond, acid waste water is 1.3-1.7 with the mass flow ratio of carbide slag slurries, and the carbide slag slurries of excess can
By almost all Fe in acid waste water3+Ionic reaction generates Fe (OH)3Precipitate.Neutralization pond can be arranged and stir
Mixing equipment, so that reaction is more abundant.
In step (1), the isolated thick solid insoluble particle diameter of cyclone hydraulic separators is below 40 mesh, removes thick solid
Body insoluble matter, follow-up the carrying out neutralizing reaction.
In described step (3), the supernatant in clean solution tank is back to slurrying groove to discharge bottom cyclone separator
Impurity carries out slurrying or is used as the cleaning mixture of chlorinated exhaust.
Step (3) described pressure filter is diaphragm filter press, precipitate underflow liquid through diaphragm filter press filter after,
Water flowing washing again, removes the solable matter in filter cake, predominantly chloride etc.；Again by diaphragm filter press supercharging
To 5.5-6.5bar, from filter cake, extrude moisture content, by compressed air, the free water in filter cake is blown out the most again
Obtaining hydroxide filter cake, filtrate goes filtrate receiver to carry out subsequent treatment.Fe (OH) in hydroxide filter cake3Account for 45%,
The unreacted Ca of excess (OH)2Account for 38%.Often produce 1 ton of Titanium Dioxide Produced by Chloride Procedure base material and about can get 0.12 ton
Hydroxide filter cake.
Described hydroxide filter cake Main Ingredients and Appearance is Fe (OH)3With Ca (OH)2, and Al (OH) in a small amount3And SiO2
Deng.The Main Ingredients and Appearance of cement: CaO:62-67%；SiO2: 20-24%；Al2O3: 4-7%；Fe2O3: 2.5-5%,
Therefore hydroxide filter cake is fully available for cement producting material.By washing, air scavenging during cake filtration,
After the ion that manufacture of cement is poisonous can being removed by the chloride ion in filter cake etc., can be used for manufacture of cement, it is achieved titanium
The comprehensive utilization of white lead waste residue.
Utilizing in generated by polyvinyl chloride by calcium carbide production process, the carbide slag slurries by-product that acetylene generation operation produces processes
The acid waste water method of Titanium Dioxide Produced by Chloride Procedure, has the refuse in titanium dioxide and two industries of generated by polyvinyl chloride by calcium carbide
Machine is combined with, it is achieved the treatment of wastes with processes of wastes against one another.The hydroxide filter cake that its reactant generates simultaneously complies fully with electricity
The cement producting material requirement of stone method vinyl chloride auxiliary construction, can be used for manufacture of cement by neutralizing waste residue.
Embodiment 1:
Carbide slag oleo stock is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation, through spinning liquid
Separator obtains carbide slag slurries and delivers to carbide slag slurries storage after isolating the particle diameter thick solid insoluble below 40 mesh
Groove；Carbide slag slurries in carbide slag slurries storage tank, through delivery pump, joins neutralization pond and is neutralized instead with acid waste water
Should, acid waste water is 1.3 with the mass flow ratio of carbide slag slurries；Neutralize reacted mixture inflow waste liquid to sink
Pond, shallow lake is precipitated, and precipitate underflow liquid is from flowing into underflow liquid storage tank, then is delivered to pressure filter by dense slurry feeding pump
Filter cake is formed after carrying out filter pressing, washing；In waste liquid sedimentation tank, supernatant is sent to clean solution tank, then is carried by clean solution tank
To slurrying groove, the impurity discharged bottom cyclone separator is carried out slurrying.
Embodiment 2:
Producing the Titanium Dioxide Produced by Chloride Procedure device of 50,000 tons per year, acid waste water generation amount is 13000kg/h；Carbide slag is former
Slurry is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation, isolates through cyclone hydraulic separators
Ca (OH) is obtained after the particle diameter thick solid insoluble below 40 mesh2Content is that the carbide slag slurries of 18-20% delivers to electricity
Rock ballast slurry storage tank；Carbide slag slurries in carbide slag slurries storage tank, through delivery pump, joins neutralization pond and enters with acid waste water
Row neutralizes reaction, and the flow of carbide slag slurries is 8666kg/h；Neutralize reacted mixture and flow into waste liquid precipitation
Pond is precipitated；In waste liquid sedimentation tank, supernatant can be sent to slurrying groove, to the impurity discharged bottom cyclone separator
Carry out slurrying；Precipitate underflow liquid is from flowing into underflow liquid storage tank, then is delivered to diaphragm filter press by dense slurry feeding pump
Carrying out filter pressing, precipitate underflow liquid is after diaphragm filter press filters, then water flowing washing in filter cake, removes filter cake
In the solable matter such as chloride, then diaphragm filter press is pressurized to about 6bar, expressed water from filter cake
Part, by compressed air, the free water in filter cake being blown out to obtain hydroxide filter cake the most again, hydroxide filter cake is used
Make to produce the raw material of cement.Filtrate after Filter Press is sent to filtrate receiver and is carried out subsequent treatment.
Embodiment 3:
Carbide slag oleo stock is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation, through spinning liquid
Separator obtains carbide slag slurries and delivers to carbide slag slurries storage after isolating the particle diameter thick solid insoluble below 40 mesh
Groove；Carbide slag slurries in carbide slag slurries storage tank, through delivery pump, joins neutralization pond and is neutralized instead with acid waste water
Should, acid waste water is 1.7 with the mass flow ratio of carbide slag slurries；Neutralize reacted mixture inflow waste liquid to sink
Pond, shallow lake is precipitated；In waste liquid sedimentation tank, supernatant is sent to clean solution tank, after be sent to chlorinated exhaust washing system conduct
The cleaning mixture of chlorinated exhaust；Precipitate underflow liquid from flow into underflow liquid storage tank, then by dense slurry feeding pump deliver to every
Filter press membrane carries out filter pressing, and precipitate underflow liquid is after diaphragm filter press filters, then water flowing washing in filter cake,
Remove the solable matter in filter cake, then diaphragm filter press is pressurized to about 6bar, expressed water from filter cake
Part, by compressed air, the free water in filter cake being blown out to obtain hydroxide filter cake the most again, hydroxide filter cake is used
Make to produce the raw material of cement.Filtrate after Filter Press is sent to filtrate receiver and is carried out subsequent treatment.
Claims (7)
1. the processing method of acid waste water in Titanium Dioxide Produced by Chloride Procedure production process, it is characterised in that include following
Step:
(1) carbide slag oleo stock is extracted out in the carbide slag stock tank of generated by polyvinyl chloride by calcium carbide factory acetylene generation operation,
After thick solid insoluble isolated by cyclone hydraulic separators, obtain carbide slag slurries deliver to carbide slag slurries storage tank；
(2) carbide slag slurries in carbide slag slurries storage tank is in delivery pump joins neutralization pond and acid waste water is carried out
And reaction；
(3) step (2) neutralize reacted mixture flow into waste liquid sedimentation tank precipitate, precipitate underflow
Liquid is from flowing into underflow liquid storage tank, then is delivered to form filter cake after pressure filter carries out filter pressing, washing by dense slurry feeding pump；
In waste liquid sedimentation tank, supernatant is sent to clean solution tank.
The process side of acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process the most according to claim 1
Method, it is characterised in that in described step (2), acid waste water is 1.3-1.7 with the mass flow ratio of carbide slag slurries.
The process side of acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process the most according to claim 1
Method, it is characterised in that in described step (1), the isolated thick solid insoluble particle diameter of cyclone hydraulic separators is 40
Below mesh.
The process side of acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process the most according to claim 1
Method, it is characterised in that in described step (3), the supernatant in clean solution tank is back to slurrying groove to cyclonic separation
The impurity discharged bottom device carries out slurrying or is used as the cleaning mixture of chlorinated exhaust.
5. according to acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process described in any one of claim 1-4
Processing method, it is characterised in that step (3) described pressure filter is diaphragm filter press.
The process side of acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process the most according to claim 5
Method, it is characterised in that precipitate underflow liquid is after diaphragm filter press filters, then water flowing washing, removes solubility
Material, then diaphragm filter press is pressurized to 5.5-6.5bar, from filter cake, extrude moisture content, the most again with compression
Free water in filter cake is blown out to obtain hydroxide filter cake by air.
The process side of acid waste water in a kind of Titanium Dioxide Produced by Chloride Procedure production process the most according to claim 6
Method, it is characterised in that described hydroxide filter cake is used as to produce the raw material of cement.
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| CN201610364216.5A CN105884082A (en) | 2016-05-26 | 2016-05-26 | Method for treating acid wastewater in titanium dioxide production process through chlorination method |
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Cited By (6)
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| CN108285233A (en) * | 2017-01-09 | 2018-07-17 | 北京水木方科技有限公司 | A kind of method of Recovery Purifying titanium white waste liquid |
| CN108585281A (en) * | 2018-05-16 | 2018-09-28 | 四川龙蟒钛业股份有限公司 | A method of reducing efflux wastewater phosphorus content |
| CN109205873A (en) * | 2018-11-20 | 2019-01-15 | 宜昌银钒科技有限公司 | A kind of wet process extracting vanadium from stone coal purifying process of waste water |
| CN111498912A (en) * | 2020-05-14 | 2020-08-07 | 河南佰利联新材料有限公司 | Resource utilization method of waste acid water produced by chlorination process |
| CN113511716A (en) * | 2021-07-12 | 2021-10-19 | 张刚 | Sewage treatment device and method for producing PVC (polyvinyl chloride) by calcium carbide method |
| CN113912234A (en) * | 2021-10-27 | 2022-01-11 | 龙佰禄丰钛业有限公司 | Method for treating sewage generated by producing titanium dioxide by chlorination process |
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Cited By (6)
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| CN113511716A (en) * | 2021-07-12 | 2021-10-19 | 张刚 | Sewage treatment device and method for producing PVC (polyvinyl chloride) by calcium carbide method |
| CN113912234A (en) * | 2021-10-27 | 2022-01-11 | 龙佰禄丰钛业有限公司 | Method for treating sewage generated by producing titanium dioxide by chlorination process |
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