CN109928434A - A method of bodied ferric sulfate is prepared with ferrous sulfate monohydrate and spent acid - Google Patents
A method of bodied ferric sulfate is prepared with ferrous sulfate monohydrate and spent acid Download PDFInfo
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- CN109928434A CN109928434A CN201910155433.7A CN201910155433A CN109928434A CN 109928434 A CN109928434 A CN 109928434A CN 201910155433 A CN201910155433 A CN 201910155433A CN 109928434 A CN109928434 A CN 109928434A
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- ferrous sulfate
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- sulfate monohydrate
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Abstract
The invention belongs to chemical industrial waste object resource utilization technical field, it is related to a kind of method that the by-product ferrous sulfate monohydrate in production process of titanium pigment and spent acid prepare water treatment agent bodied ferric sulfate.The present invention uses by-product ferrous sulfate monohydrate in production process of titanium pigment and spent acid for raw material, primes bodied ferric sulfate efficiently can quickly be produced using a small amount of catalyst, the comprehensive utilization ratio of by-product and recycling degree in production process of titanium pigment are significantly improved, is increased comprehensive economic efficiency.
Description
Technical field
The invention belongs to chemical industrial waste object resource utilization technical fields, are related to using the by-product in production process of titanium pigment
The method that object ferrous sulfate monohydrate and spent acid prepare water treatment agent bodied ferric sulfate.
Background technique
Bodied ferric sulfate is a kind of inorganic polymer flocculant of superior performance, has hydrolysis rate fast, floc density
Greatly, the features such as applicable pH range is wide.Bodied ferric sulfate morphological characters is faint yellow unformed powdery solid, is highly soluble in water,
The aqueous solution of 10% (quality) is rufous clear solution.Since bodied ferric sulfate has charge on very strong neutralization suspended particulate
Ability, have very big specific surface area and very strong adsorption capacity, can go well water removal in suspended matter, organic matter, sulfide,
The impurity such as heavy metal ion have the function of decoloration, deodorization, demulsification and sludge dewatering etc., thus be widely used in drinking water,
The purified treatment of industrial water, various industrial wastewaters, municipal sewage etc..
Many of sulfuric acid method titanium pigment production process by-product generates, wherein having a large amount of ferrous sulfate and spent acid raw
At.In waste acid concentration comprehensive utilization treatment process, ferrous sulfate by-product is caused to occur in the form of ferrous sulfate monohydrate, and surface
Containing a small amount of indissoluble ferric sulfate, it is caused to be insoluble in water, ferrous sulfate monohydrate utilization rate is very low, and effect on environment is very big.Right
Under the increasingly urgent background of comprehensive utilization of energy, more seem to the recycling comprehensive utilization process technological improvement of ferrous sulfate monohydrate
It is important.
Existing patent No. CN105129867A discloses a kind of method for preparing bodied ferric sulfate using sulfuric acid waste, still
This method is without reference to by-product of white titanium pigment ferrous sulfate monohydrate as reaction raw materials.
Existing patent No. CN109081382A discloses a kind of processing technology of bodied ferric sulfate, but this method pertain only to
Ferrous sulfate heptahydrate byproduct in titanium white production is the preparation process of raw material.
Summary of the invention
Aiming at the problems existing in the prior art, this patent is sub- using the by-product sulfuric acid monohydrate in production process of titanium pigment
Iron, spent acid are raw material, and suitable solvent is added, and the polymerised sulphur of preparation high-quality is aoxidized using sodium nitrite capsule as catalyst
Sour iron.Bodied ferric sulfate invention is achieved by following technical proposals:
(1) the by-product ferrous sulfate monohydrate solid in a certain amount of production process of titanium pigment is weighed, is put into reaction kettle, so
After be proportionally added into spent acid and water；Closed reactor is warming up to dispersion temperature, adjusts stirring rate, stirs ferrous sulfate monohydrate
Mix dispersion；
(2) it opens reaction kettle and the capsule containing catalyst sodium nitrite is added, seal reaction kettle immediately, be filled with to reaction kettle
A certain amount of oxygen increases reacting kettle inner pressure；
(3) stirring and heating are opened, reactor temperature is made to be maintained within a certain range, after reaction 70-90 minutes again
Being filled with oxygen, the reaction was continued 40-60 minutes.
(4) release processing is carried out to reaction kettle after reaction terminating, take out sample and carries out analysis test.
In step (1), the by-product ferrous sulfate monohydrate surface of solids in the production process of titanium pigment contains on a small quantity
It is insoluble in the ferric sulfate (Fe of water2(SO4)3)；The spent acid is the sulfuric acid of 20wt%.
In step (1), spent acid and ferrous sulfate monohydrate mass ratio are 1:2.5-3.0, water and ferrous sulfate monohydrate quality
Than for 1:1.1-1.3.
In step (1), the dispersion temperature is 50-60 DEG C, and stirring rate is 600-1000 revs/min, and jitter time is not
Lower than 30 minutes.
In step (2), the catalyst sodium nitrite additional amount is the 0.8%-1.2% of ferrous sulfate monohydrate quality, institute
Stating capsule is starch capsule.
In step (2) and (3), it is 2.0-2.4Mpa that oxygen, which is filled with rear pressure,.
In step (3), the reaction stirring rate is 1000-1200 revs/min, and reaction temperature maintains 90-100
DEG C, it is cooled down immediately when temperature breaks through 100 DEG C.
In step (4), determine the mark of reaction terminating for pressure it is constant and keep 30 minutes；The analysis of sample measures reference
GBT14591-2016。
The invention has the benefit that
The present invention makes full use of the by-product ferrous sulfate monohydrate of titanium dioxide to react with spent acid and suitable water, uses
A small amount of catalyst efficiently can quickly produce primes bodied ferric sulfate, greatly improve by-product in production process of titanium pigment
Comprehensive utilization ratio, increase comprehensive economic efficiency.
Specific embodiment
The following are presently preferred embodiments of the present invention, the present invention better understood when, but the embodiment of the present invention is not limited to
This, while its shown data does not represent the limitation to feature of present invention range.
Embodiment 1:
106g by-product ferrous sulfate monohydrate solid is put into reaction kettle, 40g spent acid is weighed and 82mL water pours into reaction kettle.
Closed reactor is warming up to 50 DEG C, and opening stirring and keeping revolving speed is 600 revs/min, stock dispersion 30 minutes in reaction kettle.Dispersion
After open reaction kettle be added 1.0g sodium nitrite (it is intracapsular that sodium nitrite is packed into amylan in advance), and immediately sealing reaction
Kettle.Being filled with oxygen to reaction kettle makes reacting kettle inner pressure be increased to 2.0MPa.Stirring is opened, revolving speed is 1000 revs/min, is opened
Heating, makes temperature maintain 90-100 DEG C, when temperature is more than 100 DEG C cooling in time.Reaction pressure drops after reaction carries out 90 minutes
To 1.0MPa, being filled with oxygen again makes pressure maintain 2.0MPa, and the reaction was continued after sixty minutes, and pressure maintains 1.6MPa and not
Decline again, stops reaction after the reaction was continued at this pressure 30 minutes.
180 minutes total used times are reacted in embodiment 1, are sampled and analyzed.Experimental result is shown in Table 1.
Embodiment 2:
200g by-product ferrous sulfate monohydrate solid is put into reaction kettle, 80g spent acid is weighed and 180mL water pours into reaction
Kettle.Closed reactor is warming up to 60 DEG C, and opening stirring and keeping revolving speed is 700 revs/min, stock dispersion 30 minutes in reaction kettle.
Reaction kettle is opened after dispersion, 1.6g sodium nitrite (it is intracapsular that sodium nitrite is packed into amylan in advance) is added, and sealing is anti-immediately
Answer kettle.Being filled with oxygen to reaction kettle makes reacting kettle inner pressure be increased to 2.4MPa.Stirring is opened, revolving speed is 1200 revs/min, is beaten
Heating is opened, temperature is made to maintain 90-100 DEG C, when temperature is more than 100 DEG C cooling in time.Counter-pressure drops after reaction carries out 70 minutes
To 0.8MPa, being filled with oxygen again makes pressure maintain 2.4MPa, and after the reaction was continued 50 minutes, pressure maintains 1.8MPa and not
Decline again, stops reaction after the reaction was continued at this pressure 30 minutes.
It reacts total time-consuming 150 minutes, samples and analyzes in embodiment 2.Experimental result is shown in Table 1.
Embodiment 3:
150g by-product ferrous sulfate monohydrate solid is put into reaction kettle, 55g spent acid is weighed and 115mL water pours into reaction
Kettle.Closed reactor is warming up to 50 DEG C, and opening stirring and keeping revolving speed is 900 revs/min, stock dispersion 30 minutes in reaction kettle.
Reaction kettle is opened after dispersion, 1.5g sodium nitrite (it is intracapsular that sodium nitrite is packed into amylan in advance) is added, and sealing is anti-immediately
Answer kettle.Being filled with oxygen to reaction kettle makes reacting kettle inner pressure be increased to 2.2MPa.Stirring is opened, revolving speed is 1200 revs/min, is beaten
Heating is opened, temperature is made to maintain 90-100 DEG C, when temperature is more than 100 DEG C cooling in time.Reaction pressure after reaction carries out 80 minutes
Be down to 0.9MPa, being filled with oxygen again makes pressure maintain 2.2MPa, after the reaction was continued 50 minutes, pressure maintain 1.8MPa and
No longer decline, stops reaction after the reaction was continued at this pressure 30 minutes.
160 minutes total used times are reacted in embodiment 3, are sampled and analyzed.Experimental result is shown in Table 1.
Embodiment 4:
120g by-product ferrous sulfate monohydrate solid is put into reaction kettle, 45g spent acid 105mL water is weighed and pours into reaction kettle.
Closed reactor is warming up to 60 DEG C, and opening stirring and keeping revolving speed is 1000 revs/min, stock dispersion 30 minutes in reaction kettle.Point
Reaction kettle is opened after dissipating, 1.4g sodium nitrite (it is intracapsular that sodium nitrite is packed into amylan in advance) is added, and sealing reaction immediately
Kettle.Being filled with oxygen to reaction kettle makes reacting kettle inner pressure be increased to 2.1MPa.Stirring is opened, revolving speed is 1000 revs/min, is opened
Heating, makes temperature maintain 90-100 DEG C, when temperature is more than 100 DEG C cooling in time.Reaction has carried out reaction pressure after 90 minutes
Be down to 1.1MPa, being filled with oxygen again makes pressure maintain 2.1MPa, and the reaction was continued carries out after forty minutes, pressure in 1.7MPa and
No longer decline, stops reaction after the reaction was continued at this pressure 30 minutes.
160 minutes total used times are reacted in embodiment 4, are sampled and analyzed.Experimental result is shown in Table 1.
Comparative example:
Comparative example is that traditional ferrous sulfate heptahydrate is that raw material prepares bodied ferric sulfate.
235g ferrous sulfate heptahydrate solid is put into reaction kettle together, 20% spent acid for measuring 39mL pours into reaction kettle.
Closed reactor is warming up to 40 DEG C, and opening stirring and keeping revolving speed is 600 revs/min pre- to raw material progress 30 minutes in reaction kettle
It is molten.Reaction kettle is opened after being pre-dissolved, 2.0g sodium nitrite (it is intracapsular that sodium nitrite is packed into amylan in advance) is added, and close immediately
Seal reaction kettle.Being filled with oxygen to reaction kettle makes reacting kettle inner pressure be increased to 2.0MPa.Stirring is opened, revolving speed is 1000 revs/min
Clock opens heating, temperature is made to maintain 80-90 DEG C, when temperature is more than 90 DEG C cooling in time.Reaction carries out reaction pressure after forty minutes
Power is down to 0.9MPa, and being filled with oxygen again makes pressure maintain 2.0MPa, and after continuing the reaction for 40 minutes, pressure is in 1.8MPa and not
Decline again, stops reaction after the reaction was continued at this pressure 30 minutes.
110 minutes total used times are reacted in comparative example, are sampled and analyzed.Experimental result is shown in Table 1.
1 experimental result of table:
Claims (8)
1. a kind of method for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that carry out in the steps below
:
(1) the by-product ferrous sulfate monohydrate solid in a certain amount of production process of titanium pigment is weighed, puts into reaction kettle, then presses
Spent acid and water is added in ratio；Closed reactor is warming up to dispersion temperature, adjusts stirring rate, to ferrous sulfate monohydrate stirring point
It dissipates；
(2) it opens reaction kettle and the capsule containing catalyst sodium nitrite is added, seal reaction kettle immediately, be filled with centainly to reaction kettle
The oxygen of amount increases reacting kettle inner pressure；
(3) stirring and heating are opened, reactor temperature is made to be maintained within a certain range, reaction is filled with again after 70-90 minutes
The reaction was continued 40-60 minutes for oxygen；
(4) release processing is carried out to reaction kettle after reaction terminating, take out sample and carries out analysis test.
2. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (1), the by-product ferrous sulfate monohydrate surface of solids in the production process of titanium pigment contains is insoluble in water on a small quantity
Ferric sulfate；The spent acid is the sulfuric acid of 20wt%.
3. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (1), spent acid and ferrous sulfate monohydrate mass ratio are 1:2.5-3.0, and the ratio of water and ferrous sulfate monohydrate quality is 1:
1.1-1.3。
4. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (1), the dispersion temperature is 50-60 DEG C, and stirring rate is 600-1000 revs/min, and jitter time is not less than 30 points
Clock.
5. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (2), the catalyst sodium nitrite additional amount is the 0.8%-1.2% of ferrous sulfate monohydrate quality, and the capsule is
Starch capsule.
6. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (2) and (3), it is 2.0-2.4Mpa that oxygen, which is filled with rear pressure,.
7. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (3), the reaction stirring rate is 1000-1200 revs/min, and reaction temperature maintains 90-100 DEG C, works as temperature
It is cooled down immediately when higher than 100 DEG C.
8. the method according to claim 1 for preparing bodied ferric sulfate with ferrous sulfate monohydrate and spent acid, which is characterized in that
In step (4), determine the mark of reaction terminating for pressure it is constant and keep 30 minutes；The analysis of sample measures reference
GBT14591-2016。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115215369A (en) * | 2022-08-26 | 2022-10-21 | 龙佰集团股份有限公司 | Recycling method and application of artificial rutile mother liquor |
| CN115448277A (en) * | 2022-09-06 | 2022-12-09 | 湖北融通高科先进材料有限公司 | Purification and utilization method and application of phosphorus-containing waste acid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995023765A1 (en) * | 1994-03-04 | 1995-09-08 | Imperial College Of Science, Technology & Medicine | Preparations and uses of polyferric sulphate |
| CN101434414A (en) * | 2008-12-12 | 2009-05-20 | 嘉兴市环科化工有限公司 | Preparation of polymeric ferric sulfate |
| CN104071853A (en) * | 2014-07-17 | 2014-10-01 | 广西平果锋华科技有限公司 | Method utilizing waste sulfuric acid and ferrous sulfate to produce polymeric ferric sulfate through oxygen pressurizing |
| CN105692717A (en) * | 2016-03-21 | 2016-06-22 | 广西福斯特再生资源环保科技有限公司 | Polyferric sulfate and preparation method of polyferric sulfate |
| CN106241889A (en) * | 2016-08-10 | 2016-12-21 | 浙江合众环保科技有限公司 | A kind of preparation method of solid sulphuric acid ferrum |
-
2019
- 2019-03-01 CN CN201910155433.7A patent/CN109928434A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995023765A1 (en) * | 1994-03-04 | 1995-09-08 | Imperial College Of Science, Technology & Medicine | Preparations and uses of polyferric sulphate |
| CN101434414A (en) * | 2008-12-12 | 2009-05-20 | 嘉兴市环科化工有限公司 | Preparation of polymeric ferric sulfate |
| CN104071853A (en) * | 2014-07-17 | 2014-10-01 | 广西平果锋华科技有限公司 | Method utilizing waste sulfuric acid and ferrous sulfate to produce polymeric ferric sulfate through oxygen pressurizing |
| CN105692717A (en) * | 2016-03-21 | 2016-06-22 | 广西福斯特再生资源环保科技有限公司 | Polyferric sulfate and preparation method of polyferric sulfate |
| CN106241889A (en) * | 2016-08-10 | 2016-12-21 | 浙江合众环保科技有限公司 | A kind of preparation method of solid sulphuric acid ferrum |
Non-Patent Citations (1)
| Title |
|---|
| 张力 等: "《自修复复合材料刹车片性能研究》", 30 April 2013, 北京交通大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115215369A (en) * | 2022-08-26 | 2022-10-21 | 龙佰集团股份有限公司 | Recycling method and application of artificial rutile mother liquor |
| CN115448277A (en) * | 2022-09-06 | 2022-12-09 | 湖北融通高科先进材料有限公司 | Purification and utilization method and application of phosphorus-containing waste acid |
| CN115448277B (en) * | 2022-09-06 | 2024-01-05 | 湖北融通高科先进材料集团股份有限公司 | Purification and utilization method and application of phosphorus-containing waste acid |
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