CN110479064A - A kind of preparation method of compound mercury removal agent - Google Patents
A kind of preparation method of compound mercury removal agent Download PDFInfo
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- CN110479064A CN110479064A CN201910680064.3A CN201910680064A CN110479064A CN 110479064 A CN110479064 A CN 110479064A CN 201910680064 A CN201910680064 A CN 201910680064A CN 110479064 A CN110479064 A CN 110479064A
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- removal agent
- mercury removal
- preparation
- thiosulfate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treating Waste Gases (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of preparation method of compound mercury removal agent, the specific steps are as follows: and it by fast deoxygenated aluminium powder, boehmite dry powder, lubricant and is added containing aqueous acid, is extruded into item, it is dry；Dried strip is calcined in oxidizing atmosphere, and alumina support is made；Silver nitrate aqueous solution is instilled in aqueous thiosulfate, and is stirred continuously, the place of being protected from light saves backup；By alumina support dipping with silver thiosulfate maceration extract, purge is carried out to the alumina support after dipping using carbon dioxide after taking-up, purge thickness washes, is dry, and compound mercury removal agent is made.There is suitable Kong Rong, specific surface area and active component content using mercury removal agent made from the method for the present invention, contacted with to demercuration raw material more abundant, improve the demercuration precision of mercury removal agent；The preparation process of mercury removal agent is simple to operation and participation without gas phase sulfur compound, reduces pollution of the production process to environment, also reduces production cost.
Description
Technical field
The present invention relates to environmentally friendly preparation technique field more particularly to a kind of preparation methods of compound mercury removal agent.
Background technique
In the current main non-renewable fuel such as petroleum, natural gas, it can all contain the mercury of certain content, these mercury are not
Container, pipeline can be only polluted, as one of Air Pollutants, also there is certain passive work to human health after burning
With, therefore need to carry out demercuration processing to tail gas after fuel combustion.Existing mercury removal agent is primarily present following two aspects problem: one
Aspect, the active component utilization rate in mercury removal agent is low, relatively low so as to cause demercuration precision；On the other hand, the preparation of mercury removal agent
For process by the way of multi-step impregnation, operating procedure is various, and the process is more complicated, high production cost.In addition, there is also mercury removal agents
Heap density is big, carrier specific surface area is small, the susceptible to plugging defect in duct.
Summary of the invention
Present invention seek to address that the deficiencies in the prior art, and a kind of preparation method of compound mercury removal agent is provided.
The present invention to achieve the above object, using following technical scheme:
A kind of preparation method of compound mercury removal agent, the specific steps are as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading is at uniform
Expect block, will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 950-1050 DEG C of calcining in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, system
Obtain alumina support；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate leaching is made
Stain liquid, the place of being protected from light save backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, put
It sets, is taken out after more silver thiosulfate maceration extracts are evenly distributed in alumina support, using carbon dioxide to leaching after taking-up
Alumina support after stain carries out purge, the washing of purge thickness, 80 DEG C or less dry, compound mercury removal agent is made.
Further, contain the parts by weight of 5-7 containing pure phosphoric acid, ammonium dihydrogen phosphate 3-8 parts by weight in aqueous acid in step 1.
Further, the specific surface area of fast deoxygenated aluminium powder is 250-300m in step 12/ g, pore volume 0.35-
45ml/g。
Further, fast deoxygenated aluminium powder in step 1, boehmite dry powder, lubricant mass ratio be 90-95:5-
10:2-4。
Further, alumina support specific surface area 40-60m made from step 22/ g, pore volume 0.5-0.6ml/g, can
A few bore dia 40-60nm.
Further, sulphur in the additive amount and aqueous thiosulfate of silver nitrate in the silver nitrate aqueous solution in step 3
The weight ratio of the additive amount of thiosulfate is 1:3-6.
Further, the concentration of silver ion is 0.05-0.5mol/L in silver thiosulfate maceration extract made from step 3.
Further, silver nitrate aqueous solution with the speed of 12-120ml/min instills aqueous thiosulfate in step 3
In, and be stirred with the speed of 30-300r/min.
Further, the content of elemental sulfur accounts for the 7- of compound mercury removal agent gross mass in compound mercury removal agent made from step 4
10%.
The beneficial effects of the present invention are: there is suitable Kong Rong, specific surface area using mercury removal agent made from the method for the present invention
And active component content, it is contacted with to demercuration raw material more abundant, improves the demercuration precision of mercury removal agent；The preparation of mercury removal agent
Process is simple to operation and participation without gas phase sulfur compound, reduces pollution of the production process to environment, also reduces and be produced into
This.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
A kind of preparation method of compound mercury removal agent, the specific steps are as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading is at uniform
Expect block, will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 950-1050 DEG C of calcining in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, system
Obtain alumina support；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate leaching is made
Stain liquid, the place of being protected from light save backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, put
It sets, is taken out after more silver thiosulfate maceration extracts are evenly distributed in alumina support, using carbon dioxide to leaching after taking-up
Alumina support after stain carries out purge, the washing of purge thickness, 80 DEG C or less dry, compound mercury removal agent is made.
Further, contain the parts by weight of 5-7 containing pure phosphoric acid, ammonium dihydrogen phosphate 3-8 parts by weight in aqueous acid in step 1.
Further, the specific surface area of fast deoxygenated aluminium powder is 250-300m in step 12/ g, pore volume 0.35-
45ml/g。
Further, fast deoxygenated aluminium powder in step 1, boehmite dry powder, lubricant mass ratio be 90-95:5-
10:2-4。
Further, alumina support specific surface area 40-60m made from step 22/ g, pore volume 0.5-0.6ml/g, can
A few bore dia 40-60nm.
Further, sulphur in the additive amount and aqueous thiosulfate of silver nitrate in the silver nitrate aqueous solution in step 3
The weight ratio of the additive amount of thiosulfate is 1:3-6.
Further, the concentration of silver ion is 0.05-0.5mol/L in silver thiosulfate maceration extract made from step 3.
Further, silver nitrate aqueous solution with the speed of 12-120ml/min instills aqueous thiosulfate in step 3
In, and be stirred with the speed of 30-300r/min.
Further, the content of elemental sulfur accounts for the 7- of compound mercury removal agent gross mass in compound mercury removal agent made from step 4
10%.
There is suitable Kong Rong, specific surface area and active component content using mercury removal agent made from the method for the present invention, with
It is more abundant to the contact of demercuration raw material, improve the demercuration precision of mercury removal agent；The preparation process of mercury removal agent is simple to operation and nothing
The participation of gas phase sulfur compound reduces pollution of the production process to environment, also reduces production cost.
Embodiment one
A kind of preparation method of compound mercury removal agent, the specific steps are as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading is at uniform
Expect block, will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 950 DEG C of calcinings in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, oxygen is made
Change alumina supporter；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate leaching is made
Stain liquid, the place of being protected from light save backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, put
It sets, is taken out after more silver thiosulfate maceration extracts are evenly distributed in alumina support, using carbon dioxide to leaching after taking-up
Alumina support after stain carries out purge, the washing of purge thickness, 80 DEG C or less dry, compound mercury removal agent is made.
Further, containing in step 1 contains 5 parts by weight of pure phosphoric acid, 3 parts by weight of ammonium dihydrogen phosphate in aqueous acid.
Further, the specific surface area of fast deoxygenated aluminium powder is 250m in step 12/ g, pore volume 0.35ml/g.
Further, fast deoxygenated aluminium powder in step 1, boehmite dry powder, lubricant mass ratio be 90:5:2.
Further, alumina support specific surface area 40m made from step 22/ g, pore volume 0.5ml/g, can several Kong Zhi
Diameter 40nm.
Further, sulphur in the additive amount and aqueous thiosulfate of silver nitrate in the silver nitrate aqueous solution in step 3
The weight ratio of the additive amount of thiosulfate is 1:3.
Further, the concentration of silver ion is 0.05mol/L in silver thiosulfate maceration extract made from step 3.
Further, silver nitrate aqueous solution is instilled in aqueous thiosulfate in step 3 with the speed of 12ml/min,
And it is stirred with the speed of 30r/min.
Further, the content of elemental sulfur accounts for the 7% of compound mercury removal agent gross mass in compound mercury removal agent made from step 4.
Embodiment two
A kind of preparation method of compound mercury removal agent, the specific steps are as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading is at uniform
Expect block, will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 1050 DEG C of calcinings in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, oxygen is made
Change alumina supporter；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate leaching is made
Stain liquid, the place of being protected from light save backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, put
It sets, is taken out after more silver thiosulfate maceration extracts are evenly distributed in alumina support, using carbon dioxide to leaching after taking-up
Alumina support after stain carries out purge, the washing of purge thickness, 80 DEG C or less dry, compound mercury removal agent is made.
Further, containing in step 1 contains 7 parts by weight of pure phosphoric acid, 8 parts by weight of ammonium dihydrogen phosphate in aqueous acid.
Further, the specific surface area of fast deoxygenated aluminium powder is 300m in step 12/ g, pore volume 45ml/g.
Further, fast deoxygenated aluminium powder in step 1, boehmite dry powder, lubricant mass ratio be 95:10:4.
Further, alumina support specific surface area 60m made from step 22/ g, pore volume 0.6ml/g, can several Kong Zhi
Diameter 60nm.
Further, sulphur in the additive amount and aqueous thiosulfate of silver nitrate in the silver nitrate aqueous solution in step 3
The weight ratio of the additive amount of thiosulfate is 1:6.
Further, the concentration of silver ion is 0.5mol/L in silver thiosulfate maceration extract made from step 3.
Further, silver nitrate aqueous solution is instilled in aqueous thiosulfate in step 3 with the speed of 120ml/min,
And it is stirred with the speed of 300r/min.
Further, the content of elemental sulfur accounts for compound mercury removal agent gross mass in compound mercury removal agent made from step 4
10%.
Embodiment three
A kind of preparation method of compound mercury removal agent, the specific steps are as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading is at uniform
Expect block, will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 1000 DEG C of calcinings in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, oxygen is made
Change alumina supporter；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate leaching is made
Stain liquid, the place of being protected from light save backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, put
It sets, is taken out after more silver thiosulfate maceration extracts are evenly distributed in alumina support, using carbon dioxide to leaching after taking-up
Alumina support after stain carries out purge, the washing of purge thickness, 80 DEG C or less dry, compound mercury removal agent is made.
Further, containing in step 1 contains 6 parts by weight of pure phosphoric acid, 5 parts by weight of ammonium dihydrogen phosphate in aqueous acid.
Further, the specific surface area of fast deoxygenated aluminium powder is 270m in step 12/ g, pore volume 0.4ml/g.
Further, fast deoxygenated aluminium powder in step 1, boehmite dry powder, lubricant mass ratio be 92:6:3.
Further, alumina support specific surface area 50m made from step 22/ g, pore volume 0.55ml/g, can several Kong Zhi
Diameter 50nm.
Further, sulphur in the additive amount and aqueous thiosulfate of silver nitrate in the silver nitrate aqueous solution in step 3
The weight ratio of the additive amount of thiosulfate is 1:4.
Further, the concentration of silver ion is 0.2mol/L in silver thiosulfate maceration extract made from step 3.
Further, silver nitrate aqueous solution is instilled in aqueous thiosulfate in step 3 with the speed of 50ml/min,
And it is stirred with the speed of 100r/min.
Further, the content of elemental sulfur accounts for the 9% of compound mercury removal agent gross mass in compound mercury removal agent made from step 4.
The present invention is exemplarily described above in conjunction with specific embodiment, it is clear that the present invention implements not by upper
The limitation of mode is stated, as long as using the various improvement that the inventive concept and technical scheme of the present invention carry out, or not improved straight
It scoops out for other occasions, it is within the scope of the present invention.
Claims (9)
1. a kind of preparation method of compound mercury removal agent, which is characterized in that specific step is as follows:
Step 1 prepares dried strip,
Fast deoxygenated aluminium powder, boehmite dry powder, lubricant are mixed, and is added and contains aqueous acid, kneading at equal refining block,
It will expect that block is extruded into item using the orifice plate of banded extruder, be dried to item is squeezed out, dried strip is made；
Step 2 prepares alumina support,
Dried strip 950-1050 DEG C of calcining in oxidizing atmosphere, until the water content of dried strip is fired to 5% hereinafter, oxygen is made
Change alumina supporter；
Step 3 prepares maceration extract,
Silver nitrate aqueous solution is slowly dropped into aqueous thiosulfate, and is stirred continuously, silver thiosulfate maceration extract is made,
The place of being protected from light saves backup；
Step 4, impregnated carrier,
By the dipping of alumina support made from step 2 with made from step 3 in silver thiosulfate maceration extract, it is closed, place, directly
Taken out after being evenly distributed in alumina support to more silver thiosulfate maceration extracts, after taking-up using carbon dioxide to dipping after
Alumina support carries out purge, and the washing of purge thickness is dried below 80 DEG C, and compound mercury removal agent is made.
2. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that contain aqueous acid in step 1
In the parts by weight of 5-7 containing pure phosphoric acid, ammonium dihydrogen phosphate 3-8 parts by weight.
3. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that fast deoxygenated aluminium powder in step 1
Specific surface area be 250-300m2/ g, pore volume 0.35-45ml/g.
4. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that fast deoxygenated aluminium in step 1
Powder, boehmite dry powder, lubricant mass ratio be 90-95:5-10:2-4.
5. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that carrying alumina made from step 2
Surface area per unit volume accumulates 40-60m2/ g, pore volume 0.5-0.6ml/g, can a few bore dia 40-60nm.
6. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that the silver nitrate in step 3 is water-soluble
The weight ratio of the additive amount of thiosulfate is 1:3-6 in the additive amount and aqueous thiosulfate of silver nitrate in liquid.
7. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that thiosulfuric acid made from step 3
The concentration of silver ion is 0.05-0.5mol/L in silver-colored maceration extract.
8. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that silver nitrate aqueous solution in step 3
It is instilled in aqueous thiosulfate with the speed of 12-120ml/min, and is stirred with the speed of 30-300r/min.
9. the preparation method of compound mercury removal agent according to claim 1, which is characterized in that compound demercuration made from step 4
The content of elemental sulfur accounts for the 7-10% of compound mercury removal agent gross mass in agent.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2004132179A (en) * | 2004-11-05 | 2006-04-10 | Владимир Николаевич Тимошин (RU) | METHOD FOR DISCONTINUING MERCURY CONTAINING LUMINOPHOR |
| CN104645928A (en) * | 2013-11-25 | 2015-05-27 | 北京三聚环保新材料股份有限公司 | Method for preparing silver mercury removing agent |
| CN109126413A (en) * | 2018-08-29 | 2019-01-04 | 山东迅达化工集团有限公司 | Prepare sulphur/aluminium oxide mercury removal agent method of macropore |
-
2019
- 2019-07-26 CN CN201910680064.3A patent/CN110479064A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2004132179A (en) * | 2004-11-05 | 2006-04-10 | Владимир Николаевич Тимошин (RU) | METHOD FOR DISCONTINUING MERCURY CONTAINING LUMINOPHOR |
| CN104645928A (en) * | 2013-11-25 | 2015-05-27 | 北京三聚环保新材料股份有限公司 | Method for preparing silver mercury removing agent |
| CN109126413A (en) * | 2018-08-29 | 2019-01-04 | 山东迅达化工集团有限公司 | Prepare sulphur/aluminium oxide mercury removal agent method of macropore |
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Application publication date: 20191122 |