CN109351326A - A kind of renewable mercury removal agent and preparation method thereof for natural gas - Google Patents
A kind of renewable mercury removal agent and preparation method thereof for natural gas Download PDFInfo
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- CN109351326A CN109351326A CN201811555029.0A CN201811555029A CN109351326A CN 109351326 A CN109351326 A CN 109351326A CN 201811555029 A CN201811555029 A CN 201811555029A CN 109351326 A CN109351326 A CN 109351326A
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- natural gas
- removal agent
- mercury
- mercury removal
- renewable
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
Abstract
The renewable mercury removal agent and preparation method thereof that the invention discloses a kind of for natural gas, belongs to natural gas purification field.The present invention by forming molecular screen primary powder, binder and water after mixing, screened, polishing, dry, calcining, which obtain, forms intermediate product, lye is then added and carries out crystallization, silver salt solution uniform load active component is added after washed, dry, and the product with silver for demercuration active component is most made through drying, activation afterwards.The preparation method is simple, and silver-colored utilization rate is high, and without vulcanisation step, secondary pollution is not present；Ordered molecular sieve structure is converted by binder using crystallization steps, effectively improves product strength and its suction mercury rate and efficiency to Trace Mercury in natural gas；Mercury removal agent regeneration effect is good, compared with non-renewable type mercury removal agent, can regenerate the subsequent processing for using and avoiding mercurous dangerous waste；After renewable mercury removal agent processing of the invention, mercury content≤10ng/Nm of purified natural gas3。
Description
Technical field
The invention belongs to natural gas purification fields, and in particular to a kind of renewable mercury removal agent and its system for natural gas
Preparation Method.
Background technique
Natural gas to China's energy structure optimizing and realizes carbon emission reduction target as a kind of efficient, clean green energy resource
It is of great significance.According to the difference of geological conditions, the natural gas largely produced both at home and abroad is more or less to be contained again
Mercury metal, content are generally 1000 ~ 200000ng/m3, the country also has the natural gas mercury content of some areas to be more than
1000000ng/m3.In the subsequent processing process of natural gas, mercury can be caused cryogenic heat exchange equipment, instrument and pipeline etc. seriously
Corrosion, once corrosion leakage easily causes serious production accident, the mercury in addition deposited in device can be to operator and maintenance
Worker causes personal safety to threaten problem, and natural gas as the mercury after fuel combustion enter atmosphere also and will will cause it is serious
Mercury environmental pollution.In consideration of it, to guarantee natural gas following process, conveying and the safety utilized, it is necessary to by the huge sum of money in natural gas
Belong to mercury effectively to be removed.
For the removing of Hg in natural gas, absorption method demercuration is mainly used in engineering.According to the difference of absorption principle, divide
For non-renewable demercuration and renewable demercuration technology, the former using sulfur loading active carbon or supported metal sulphide aluminium oxide as adsorbent,
The latter is using silver molecular sieve as adsorbent.Corresponding chemical reaction mechanism is as follows.
Compared with non-renewable demercuration, renewable demercuration can recycle while removing Hg in natural gas obtains liquid
Mercury product, and renewable mercury removal agent reaches hardly mercurous after service life, does not need extra process, and non-renewable mercury removal agent
Adsorption of Mercury needs to be further processed as mercurous dangerous waste after reaching service life, to handling, storage, transport and treatment process compared with
It is complicated.Therefore develop it is a kind of efficiently renewable mercury removal agent for natural gas purification technical level promotion be of great significance.
Chinese patent CN104645927A discloses a kind of preparation method of silver system mercury removal agent, with silver ammonia complex solution
It is impregnated on carrier, then the mercury removal agent that active component is silver sulfide is made through vulcanizing, which needs using vulcanizing agent, sulphur
Change process is complicated, and there is also secondary pollution problems for superfluous sulfide solution, and it still falls within metal sulfide type
Non-renewable type mercury removal agent, silver-colored price is relatively expensive, does not only have industrial application value substantially as disposable.It is Chinese special
Silver disclosed in sharp CN104645928A is the preparation method of mercury removal agent, and belongs to the non-renewable type that active component is silver sulfide
Type mercury removal agent, equally exists the above problem.
Summary of the invention
For various disadvantages existing for above-mentioned existing natural gas mercury-removing agent, the present invention is intended to provide a kind of preparation process is simple
It is single, it is that demercuration active component produces renewable High-efficiency Gas mercury removal agent without vulcanization at low cost with silver.
To achieve the above object, this invention takes following technical schemes:
A kind of renewable mercury removal agent for natural gas, be by by molecular screen primary powder, binder and water after mixing at
Type, screened, polishing, dry, calcining, which obtain, forms intermediate product, and lye is then added and carries out crystallization, it is washed, dry after again plus
Enter silver salt solution uniform load active component, most afterwards through final products obtained by drying, activation.
The renewable mercury removal agent it is specific the preparation method comprises the following steps:
(1) molecular screen primary powder, binder and water are formed on nodulizer or banded extruder after mixing；
(2) it is obtained after forming through screening, polishing, drying, calcining and forms intermediate product；
(3) intermediate product will be formed, lye progress crystallization is added, the binder with disordered structure is made to be converted into ordered molecular sieve knot
Structure；
(4) it is washed with water to after crystallization neutral and dry；
(5) silver salt solution is added and carries out active component uniform load；
(6) it is taken out from silver salt solution after loading, obtains final products through drying, activation.
Further, the molecular screen primary powder is one or both of LTA type molecular sieve, FAU type molecular sieve.
Further, the binder is one or both of kaolin, boehmite, waterglass.
Further, the mass ratio of the molecular screen primary powder and binder is 1:0.1 ~ 1:0.3.
Further, the lye is the water of the mixture of sodium hydroxide, potassium hydroxide or sodium hydroxide and potassium hydroxide
Solution, concentration of lye are 1.0 ~ 4.0mol/L.
Further, the silver salt solution is the aqueous solution of silver nitrate, and silver salt molar concentration is 0.05 ~ 1.0mol/L.
Further, the temperature of the drying is 80 ~ 150 DEG C, and drying time is 1 ~ 8h.
Further, the temperature of the calcining is 450 ~ 650 DEG C, and calcination time is 2 ~ 6h.
Further, the temperature of the crystallization is 80 ~ 110 DEG C, 1 ~ 8h of crystallization time.
Further, the temperature of the load is 20 ~ 90 DEG C, 1 ~ 4h of load time.
Further, the temperature of the activation is 300 ~ 500 DEG C, and activation time is 2 ~ 6h.
Further, the silver content of the product (the renewable mercury removal agent for natural gas) is 0.1 ~ 10wt%.
Further, the regeneration temperature of the product (the renewable mercury removal agent for natural gas) is 230 ~ 320 DEG C, then
Raw 2 ~ 8h of time.
The invention has the following advantages that
(1) renewable natural gas mercury-removing agent preparation process of the invention is simple, and silver-colored utilization rate is high, without vulcanisation step, does not deposit
In secondary pollution；
(2) ordered molecular sieve structure is converted by the disordered structure of binder using crystallization steps, can not only increases molecular sieve and contains
Amount, and binder plug-hole is avoided, improve product strength and its suction mercury rate and efficiency to Trace Mercury in natural gas；
(3) natural gas mercury-removing agent made from, regeneration effect is good, compared with non-renewable type mercury removal agent, can regenerate use and
Avoid the subsequent processing of mercurous dangerous waste；
(4) after using renewable natural gas mercury-removing agent processing of the invention, mercury content≤10ng/Nm of purified natural gas3, reach
To depth demercuration technical requirements.
Specific embodiment
Below by specific embodiment, present invention is further described in detail.
Embodiment 1
LTA type molecular screen primary powder is uniformly mixed with Kaolin binder 1:0.2 in mass ratio, suitable quantity of water is sprayed into, in nodulizer
Upper roller forming is sieved after molding, polishes the bead for obtaining that partial size is 1.6 ~ 2.5mm, bead is dried 2h at 120 DEG C,
Then bead calcining 3h is obtained at 550 DEG C and forms intermediate product, it is 2.5mol/ which, which is added naoh concentration,
Neutrality and the dry 2h at 120 DEG C are washed with water in the lye of L after 95 DEG C of crystallization 5h, crystallization, then is added into silver nitrate
Concentration is to take out in 80 DEG C of dry 3h, finally activate in 400 DEG C in 60 DEG C of uniform load 2h in the silver salt solution of 0.20mol/L
Final products are made in 3h.Silver content of the product through XRF elemental analysis is 2.96wt%, is 300 μ g/Nm for mercury content3It is natural
The dynamic demercuration of gas is tested, and purified natural gas mercury content is lower than 10ng/Nm3, mercury removal agent is heated to 260 DEG C after Adsorption of Mercury
And 3h is kept, regeneration rate 99.6%, absorption and regeneration effect are good.
Embodiment 2
LTA type molecular screen primary powder is uniformly mixed with Kaolin binder 1:0.2 in mass ratio, suitable quantity of water is sprayed into, in nodulizer
Upper roller forming is sieved after molding, polishes the bead for obtaining that partial size is 1.6 ~ 2.5mm, bead is dried 2h at 120 DEG C,
Then bead calcining 3h is obtained at 550 DEG C and forms intermediate product, which is added sodium hydroxide and concentration of potassium hydroxide
Be neutrality and the dry 2h at 120 DEG C are washed with water in the lye of 1.5mol/L after 95 DEG C of crystallization 5h, crystallization, then by its
Be added in the silver salt solution that silver nitrate concentration is 0.30mol/L in 80 DEG C of uniform load 2h, take out in 80 DEG C of dry 3h, finally in
Final products are made in 400 DEG C of activation 3h.Silver content of the product through XRF elemental analysis is 4.15wt%, is 300 μ g/ for mercury content
Nm3Natural gas dynamic demercuration test, purified natural gas mercury content be lower than 10ng/Nm3, mercury removal agent is added after Adsorption of Mercury
Heat is to 280 DEG C and keeps 3h, regeneration rate 99.5%, and absorption and regeneration effect are good.
Embodiment 3
FAU type molecular screen primary powder and Kaolin binder 1:0.25 in mass ratio are uniformly mixed, suitable quantity of water is sprayed into, in nodulizer
Upper roller forming is sieved after molding, polishes the bead for obtaining that partial size is 1.6 ~ 2.5mm, bead is dried 2h at 120 DEG C,
Then bead calcining 3h is obtained at 550 DEG C and forms intermediate product, which is added sodium hydroxide and concentration of potassium hydroxide
Be neutrality and the dry 2h at 120 DEG C are washed with water in the lye of 1.5mol/L after 95 DEG C of crystallization 6h, crystallization, then by its
Be added in the silver salt solution that silver nitrate concentration is 0.30mol/L in 80 DEG C of uniform load 2h, take out in 80 DEG C of dry 3h, finally in
Final products are made in 400 DEG C of activation 3h.Silver content of the product through XRF elemental analysis is 4.38wt%, is 300 μ g/ for mercury content
Nm3Natural gas dynamic demercuration test, purified natural gas mercury content be lower than 10ng/Nm3, mercury removal agent is added after Adsorption of Mercury
Heat is to 280 DEG C and keeps 3h, regeneration rate 99.3%, and absorption and regeneration effect are good.
Above-described embodiment is only representative example of the invention, the implementation and power being not intended to limit the invention
Sharp range, all technical solutions identical or equivalent with content described in the claims in the present invention should all be included in present invention protection model
In enclosing.
Claims (10)
1. a kind of renewable mercury removal agent for natural gas, be by by molecular screen primary powder, binder and water after mixing
It forms, screened, polishing, dry, calcining obtain the intermediate product of molding, and lye is then added and carries out crystallization, after washed, drying again
Silver salt solution uniform load active component is added, most afterwards through final products obtained by drying, activation.
2. a kind of preparation method of the renewable mercury removal agent for natural gas, it is characterised in that: method includes the following steps:
(1) molecular screen primary powder, binder and water are formed on nodulizer or banded extruder after mixing；
(2) it is obtained after forming through screening, polishing, drying, calcining and forms intermediate product；
(3) intermediate product will be formed, lye progress crystallization is added, the binder with disordered structure is made to be converted into ordered molecular sieve knot
Structure；
(4) it is washed with water to after crystallization neutral and dry；
(5) silver salt solution is added and carries out active component uniform load；
(6) it is taken out from silver salt solution after loading, obtains final products through drying, activation.
3. according to the method described in claim 2, it is characterized by: the molecular screen primary powder is LTA type molecular sieve, FAU type point
One or both of son sieve；The binder is one or both of kaolin, boehmite, waterglass.
4. according to the method described in claim 2, it is characterized by: the mass ratio of the molecular screen primary powder and binder is 1:
0.1~1:0.3。
5. according to the method described in claim 2, it is characterized by: the lye is sodium hydroxide, potassium hydroxide or hydroxide
The aqueous solution of the mixture of sodium and potassium hydroxide, concentration of lye are 1.0 ~ 4.0mol/L.
6. according to the method described in claim 2, silver salt rubs it is characterized by: the silver salt solution is the aqueous solution of silver nitrate
Your concentration is 0.05 ~ 1.0mol/L.
7. according to the method described in claim 2, it is characterized by: the temperature of the drying be 80 ~ 150 DEG C, drying time 1
~8h；The temperature of the calcining is 450 ~ 650 DEG C, and calcination time is 2 ~ 6h；The temperature of the crystallization is 80 ~ 110 DEG C, when crystallization
Between 1 ~ 8h.
8. according to the method described in claim 2, it is characterized by: the temperature of the load be 20 ~ 90 DEG C, load time 1 ~
4h；The temperature of the activation is 300 ~ 500 DEG C, and activation time is 2 ~ 6h.
9. according to the method described in claim 2, it is characterized by: the silver content of the product is 0.1 ~ 10wt%.
10. the renewable mercury removal agent according to claim 1 for natural gas, it is characterised in that: this is used for natural gas
Renewable mercury removal agent regeneration temperature be 230 ~ 320 DEG C, the reproduction time be 2 ~ 8h.
Priority Applications (1)
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| CN201811555029.0A CN109351326A (en) | 2018-12-19 | 2018-12-19 | A kind of renewable mercury removal agent and preparation method thereof for natural gas |
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| CN201811555029.0A CN109351326A (en) | 2018-12-19 | 2018-12-19 | A kind of renewable mercury removal agent and preparation method thereof for natural gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193397A (en) * | 2022-07-22 | 2022-10-18 | 润和科华催化剂(上海)有限公司 | Shell silver mercury remover and preparation method thereof |
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