CN107986243A - Concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide - Google Patents
Concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide Download PDFInfo
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- CN107986243A CN107986243A CN201711218591.XA CN201711218591A CN107986243A CN 107986243 A CN107986243 A CN 107986243A CN 201711218591 A CN201711218591 A CN 201711218591A CN 107986243 A CN107986243 A CN 107986243A
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- sulfuric acid
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- acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/901—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/88—Concentration of sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide, belong to sulphuric acid concentration field, including precipitation pretreatment, flash distillation pretreatment, primary flash crystallization concentrating and separating and secondary vacuum are concentrated by evaporation four steps；Step is precipitated pretreated filtrate by the flash distillation pretreatment, is first passed through pipeline to mixing channel, is then pumped to combination cyclone separator by feed pump and carry out concentration.Spent acid Concentrated Acid Methods of the present invention, can effectively reduce ferrous sulfate content in sulfuric acid solution, improve the purity of sulfuric acid solution.The present invention is entered in injector by extraneous middle pressure steam, is formed negative pressure by 1st effective evaporator, is improved evaporation efficiency, mitigate equipment equipment corrosion, greatly improve running efficiency of system.
Description
Technical field
The present invention relates to concentrated sulfuric acid method for concentration, and in particular to concentrated sulfuric acid concentration side is produced in sulfuric acid process preparing titanium dioxide
Method.
Background technology
In sulfuric acid method titanium pigment production process, produce substantial amounts of concentration for 20% or so spent acid (in terms of H2SO4, under
Together), often produce one ton of titanium dioxide and about produce 6~8 tons of spent acid, this part spent acid will cause a large amount of treasured if do not recycled
The waste of your resource, if environment can be caused to seriously endanger (such as directly discharge) by dealing with improperly.Concentration reuse is carried out to spent acid,
It is currently to solve one of spent acid comprehensive utilization and the most effective approach of energy conservation and environmental protection.It is existing to be divided to two sections of progress for waste acid concentration
Concentration, i.e. flue gas concentration systems and steam concentration systems.Flue gas concentration systems are left to concentration 20% using rotary kiln fume afterheat
Right spent acid carries out initial concentration, and concentration brings up to 30% or so；Steam concentration systems are to lead to the spent acid of concentration 30% or so
Cross two effects and be concentrated into 60~65% or so, filtrate time production process directly utilizes after separation of solid and liquid, saves fresh sulfuric acid dosage, drop
Low product acid consumption.
Existing titanium pigment waste acid concentration technique is in the waste acid concentration stage, with the increase of acid concentration, sulfate in solution
Easily crystallization separates out so that fouling of heat exchangers and line clogging, cause utilization rate of equipment and installations low, the cycle of operation is short.The patent No.：
201010561886.9 disclose the technique that sulfuric acid and sulfate are recycled from the spent acid of method for producing gtitanium dioxide with sulphuric acid.It is special at this
In profit, specific recovery process is divided into four steps, is respectively：Precipitation pretreatment, one section of separation of " flash distillation-crystallization " concentrated acid, two
Section vacuum evaporation and three-level vacuum evaporation.Except precipitation pre-processes, there is the step of the evaporative crystallization concentration of three-level
Suddenly, technological process is excessively cumbersome；In addition, there is heating unit in each step, the energy of consumption is excessive.
The content of the invention
The present invention needs to solve the problems, such as above-mentioned be directed to, there is provided concentrated sulfuric acid concentration side is produced in sulfuric acid process preparing titanium dioxide
Method.
The manufacture method of concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide, is included the following steps：
Step 1：Spent acid is first passed through pipeline and is sent into inclined plate sedimentation pond, precipitation pretreatment is carried out, isolates coarse grain sulfuric acid
Salt；The supernatant liquor of settling tank is pipelined in diaphragm filter press, then is separated by filtration, it is thinner to isolate particle
Sulfate, crystallization tank is sent to by belt conveyor to the fine grained sulfate isolated；
Step 2：By filtrate of the step 1 after diaphragm filter press filters, pipeline is first passed through into mixing channel, Ran Houtong
Cross feed pump and pump to combination cyclone separator progress concentration；
Step 3：The filtrate of step 2 is delivered to one by sour storage tank and feed pump among the sour storage tank in the first centre, second
Imitate in evaporator；
Step 4：One effect heater is heated by low-pressure steam, reaches the temperature needed for spent acid evaporation, in 1st effective evaporator
Waste liquid, by one effect circulating pump, 1st effective evaporator and one effect heater in closed cycle, evaporate moisture content, improve spent acid
Concentration, the indirect steam produced in 1st effective evaporator, extraneous vacuum pump is followed by by condenser cooling；
Step 5：The spent acid in step 4 is pumped to level-one vaporization chamber by feed pump to be flashed, the absolute pressure of flash distillation
Power is sent to the first condenser the vapor flashed off through piping for 25KPa becomes condensate liquid after cooling water condensation
Collected with other incoagulable gas by condensed water collecting device and waste gas collection device；Supersaturated solution after flash distillation is passed through
Pipeline sets first degree crystalline room temperature as 70 DEG C, carries out level-one knot after crystallizing 50 minutes, 50 minutes to first degree crystalline room
Brilliant room temperature drops to 35 DEG C and continues crystallization 50 minutes at once；To the consolidating containing bulky grain vitriol of first degree crystalline room bottom
Liquid mixture, is pipelined in Primary diaphragm filter press, is separated by filtration, isolate vitriol；To separation
The vitriol gone out is transported to crystallization tank by belt conveyor；Filtrate after being filtered to Primary diaphragm filter press passes through pipeline
Primary heater is pumped into by first circulation to be heated for 135 DEG C of steam with temperature, the temperature of circulation fluid is reached 130
℃；Then level-one vaporization chamber that acid after heating is sent back to vacuum by pipeline again continues to flash；
Step 6：, the filtrate after the filtering of step 5 Primary diaphragm filter press is pumped into second by pipeline through second circulation
Heater is heated with temperature for 120 DEG C of steam, and recycle acid is heated to 110 DEG C；Then the acid after second is heated again
It is sent into secondary evaporimeter to be evaporated in vacuo, the absolute pressure of vacuum evaporation is 3KPa, and evaporating temperature is 100 DEG C；Two level is steamed
The vapor that hair device evaporates is sent to the second condenser through piping not to coagulate after cooling water condensation as condensate liquid with other
Property gas, pass through condensed water collecting device and waste gas collection device again for obtained condensate liquid in the second condenser and collect；
Secondary crystallization room is pipelined to the supersaturated solution after flash distillation, secondary crystallization room temperature is set as 35 DEG C, is tied
It is 40 minutes brilliant, first degree crystalline room temperature is dropped to 3 DEG C at once after forty minutes and continues crystallization 40 minutes；To secondary crystallization room bottom
Solidliquid mixture containing bulky grain vitriol, is pipelined in secondary diaphragm filter press, is separated by filtration,
Isolate vitriol；Filtrate after filtering is sent into holding tank by pipeline；
Step 7：The filtrate of holding tank filtrate is carried out high temperature evaporation steam by 110 DEG C of high temperature furnace, after evaporation
High-concentration waste liquid is passed through product holding tank.
In such scheme, the injector preferably connected on the 1st effective evaporator is sprayed using extraneous middle pressure steam
Penetrate or low-pressure steam is sprayed.
Beneficial effects of the present invention：
During the method for the invention waste acid concentration, beginning sulfuric acid concentration is small, ferrous sulfate content in sulfuric acid solution
More, using 75 degree or 35 degree of crystalline rate highests, with the increase of sulfuric acid solution concentration, ferrous sulfate contains in sulfuric acid solution
The reduction of amount, at 0 degree, ferrous sulfate is almost not dissolved in sulfuric acid solution, and 0 degree is crystallized, and can effectively reduce sulfuric acid solution
Middle ferrous sulfate content, improves the purity of sulfuric acid solution.The pre- place of increase flash distillation before primary flash crystallizes concentrating and separating step
Reason, can concentrate sulfuric acid solution.
Improve the concentration of sulfuric acid solution.
Embodiment
Embodiment shown below is described further technical scheme.
Concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide, is made of the raw material of following ratio of weight and number, including
Following steps：
Step 1：Spent acid is first passed through pipeline and is sent into inclined plate sedimentation pond, precipitation pretreatment is carried out, isolates coarse grain sulfuric acid
Salt；The supernatant liquor of settling tank is pipelined in diaphragm filter press, then is separated by filtration, it is thinner to isolate particle
Sulfate, crystallization tank is sent to by belt conveyor to the fine grained sulfate isolated.
Step 2：By filtrate of the step 1 after diaphragm filter press filters, pipeline is first passed through into mixing channel, Ran Houtong
Cross feed pump and pump to combination cyclone separator progress concentration；
Step 3：The filtrate of step 2 is delivered to one by sour storage tank and feed pump among the sour storage tank in the first centre, second
Imitate in evaporator.
Step 4：One effect heater is heated by low-pressure steam, reaches the temperature needed for spent acid evaporation, in 1st effective evaporator
Waste liquid, by one effect circulating pump, 1st effective evaporator and one effect heater in closed cycle, evaporate moisture content, improve spent acid
Concentration, the indirect steam produced in 1st effective evaporator, extraneous vacuum pump is followed by by condenser cooling.
Step 5：The spent acid in step 4 is pumped to level-one vaporization chamber by feed pump to be flashed, the absolute pressure of flash distillation
Power is sent to the first condenser the vapor flashed off through piping for 25KPa becomes condensate liquid after cooling water condensation
Collected with other incoagulable gas by condensed water collecting device and waste gas collection device；Supersaturated solution after flash distillation is passed through
Pipeline sets first degree crystalline room temperature as 70 DEG C, carries out level-one knot after crystallizing 50 minutes, 50 minutes to first degree crystalline room
Brilliant room temperature drops to 35 DEG C and continues crystallization 50 minutes at once；To the consolidating containing bulky grain vitriol of first degree crystalline room bottom
Liquid mixture, is pipelined in Primary diaphragm filter press, is separated by filtration, isolate vitriol.To separation
The vitriol gone out is transported to crystallization tank by belt conveyor；Filtrate after being filtered to Primary diaphragm filter press passes through pipeline
Primary heater is pumped into by first circulation to be heated for 135 DEG C of steam with temperature, the temperature of circulation fluid is reached 130
℃；Then level-one vaporization chamber that acid after heating is sent back to vacuum by pipeline again continues to flash.
Step 6：, the filtrate after the filtering of step 5 Primary diaphragm filter press is pumped into second by pipeline through second circulation
Heater is heated with temperature for 120 DEG C of steam, and recycle acid is heated to 110 DEG C；Then the acid after second is heated again
It is sent into secondary evaporimeter to be evaporated in vacuo, the absolute pressure of vacuum evaporation is 3KPa, and evaporating temperature is 100 DEG C.Two level is steamed
The vapor that hair device evaporates is sent to the second condenser through piping not to coagulate after cooling water condensation as condensate liquid with other
Property gas, pass through condensed water collecting device and waste gas collection device again for obtained condensate liquid in the second condenser and collect；
Secondary crystallization room is pipelined to the supersaturated solution after flash distillation, secondary crystallization room temperature is set as 35 DEG C, is tied
It is 40 minutes brilliant, first degree crystalline room temperature is dropped to 3 DEG C at once after forty minutes and continues crystallization 40 minutes；To secondary crystallization room bottom
Solidliquid mixture containing bulky grain vitriol, is pipelined in secondary diaphragm filter press, is separated by filtration,
Isolate vitriol；Filtrate after filtering is sent into holding tank by pipeline.
Step 7：The filtrate of holding tank filtrate is carried out high temperature evaporation steam by 110 DEG C of high temperature furnace, after evaporation
High-concentration waste liquid is passed through product holding tank.
The preferred embodiment to the invention is illustrated above, but the present invention is not limited to embodiment,
Those skilled in the art can also make a variety of equivalent modifications on the premise of without prejudice to the invention spirit
Or replace, these equivalent modifications or replacement are all contained in scope of the present application.
Claims (2)
1. the manufacture method of concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide, it is characterised in that：Include the following steps：
Step 1：Spent acid is first passed through pipeline and is sent into inclined plate sedimentation pond, precipitation pretreatment is carried out, isolates coarse grain sulfate；It is right
The supernatant liquor of settling tank is pipelined in diaphragm filter press, then is separated by filtration, and isolates the thinner sulphur of particle
Hydrochlorate, crystallization tank is sent to the fine grained sulfate isolated by belt conveyor；
Step 2：By filtrate of the step 1 after diaphragm filter press filters, first pass through pipeline into mixing channel, then by into
Material pumping is sent to combination cyclone separator and carries out concentration；
Step 3：The filtrate of step 2 is delivered to an effect by sour storage tank and feed pump among the sour storage tank in the first centre, second to steam
Send out in device；
Step 4：One effect heater is heated by low-pressure steam, reaches the temperature needed for spent acid evaporation, in 1st effective evaporator
Waste liquid, by an effect circulating pump, the closed cycle in 1st effective evaporator and an effect heater, evaporates moisture content, improves acid-spending strength,
The indirect steam produced in 1st effective evaporator, extraneous vacuum pump is followed by by condenser cooling；
Step 5：The spent acid in step 4 is pumped to level-one vaporization chamber by feed pump to be flashed, the absolute pressure of flash distillation is
25KPa send to the first condenser the vapor flashed off through piping becomes condensate liquid and its after cooling water condensation
He is collected incoagulable gas by condensed water collecting device and waste gas collection device；Pipeline is passed through to the supersaturated solution after flash distillation
First degree crystalline room is transported to, sets first degree crystalline room temperature as 70 DEG C, is carried out first degree crystalline room after crystallizing 50 minutes, 50 minutes
Temperature drops to 35 DEG C and continues crystallization 50 minutes at once；The solid-liquid containing bulky grain vitriol of first degree crystalline room bottom is mixed
Compound, is pipelined in Primary diaphragm filter press, is separated by filtration, isolate vitriol；To what is isolated
Vitriol is transported to crystallization tank by belt conveyor；Filtrate after being filtered to Primary diaphragm filter press is passed through by pipeline
First circulation is pumped into primary heater and is heated with temperature for 135 DEG C of steam, the temperature of circulation fluid is reached 130 DEG C；So
The level-one vaporization chamber that acid after heating is sent back to vacuum by pipeline again afterwards continues to flash；
Step 6：, the filtrate after the filtering of step 5 Primary diaphragm filter press is pumped into the second heating by pipeline through second circulation
Device is heated with temperature for 120 DEG C of steam, and recycle acid is heated to 110 DEG C；Then the acid after second is heated again is sent into
Secondary evaporimeter is evaporated in vacuo, and the absolute pressure of vacuum evaporation is 3KPa, and evaporating temperature is 100 DEG C；To secondary evaporimeter
The vapor evaporated is sent to the second condenser through piping becomes condensate liquid and other incoagulability gas after cooling water condensation
Body, is collected by condensed water collecting device and waste gas collection device again for obtained condensate liquid in the second condenser；To dodging
Supersaturated solution after steaming is pipelined to secondary crystallization room, sets secondary crystallization room temperature as 35 DEG C, carries out crystallization 40
Minute, first degree crystalline room temperature is dropped to 3 DEG C at once after forty minutes and continues crystallization 40 minutes；Secondary crystallization room bottom is contained
The solidliquid mixture of bulky grain vitriol, is pipelined in secondary diaphragm filter press, is separated by filtration, separation
Go out vitriol；Filtrate after filtering is sent into holding tank by pipeline；
Step 7：The filtrate of holding tank filtrate is carried out high temperature evaporation steam by 110 DEG C of high temperature furnace, highly concentrated after evaporation
Degree waste liquid is passed through product holding tank.
2. producing the manufacture method of concentrated sulfuric acid method for concentration in sulfuric acid process preparing titanium dioxide according to claim 1, it is special
Sign is：The injector connected on the 1st effective evaporator is sprayed using extraneous middle pressure steam or low-pressure steam is sprayed
Penetrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711218591.XA CN107986243A (en) | 2017-11-28 | 2017-11-28 | Concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide |
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| CN201711218591.XA CN107986243A (en) | 2017-11-28 | 2017-11-28 | Concentrated sulfuric acid method for concentration is produced in sulfuric acid process preparing titanium dioxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111924808A (en) * | 2020-09-09 | 2020-11-13 | 胡光雄 | Equipment for concentrating high-temperature flue gas waste acid in titanium dioxide production by sulfuric acid method and use method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774816A (en) * | 2012-08-02 | 2012-11-14 | 潜江方圆钛白有限公司 | Method and device for concentrating waste acid in titanium dioxide production by sulfuric acid process |
| CN105883730A (en) * | 2016-05-05 | 2016-08-24 | 中钛集团洛阳市裕星化工有限公司 | Method for concentrating waste acid in titanium dioxide production based on sulfuric acid process |
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- 2017-11-28 CN CN201711218591.XA patent/CN107986243A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774816A (en) * | 2012-08-02 | 2012-11-14 | 潜江方圆钛白有限公司 | Method and device for concentrating waste acid in titanium dioxide production by sulfuric acid process |
| CN105883730A (en) * | 2016-05-05 | 2016-08-24 | 中钛集团洛阳市裕星化工有限公司 | Method for concentrating waste acid in titanium dioxide production based on sulfuric acid process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111924808A (en) * | 2020-09-09 | 2020-11-13 | 胡光雄 | Equipment for concentrating high-temperature flue gas waste acid in titanium dioxide production by sulfuric acid method and use method |
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Application publication date: 20180504 |