CN106925229A - A kind of iron zinc-base wood composite quality activated carbon desulphurization agent and preparation method thereof - Google Patents
A kind of iron zinc-base wood composite quality activated carbon desulphurization agent and preparation method thereof Download PDFInfo
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- B01J20/0229—Compounds of Fe
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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Abstract
The invention discloses a kind of iron zinc-base wood composite quality activated carbon desulphurization agent and preparation method thereof, using the lignin of masson pine black liquid extraction by obtaining Lignin Activated Carbon after carbonization-activation, Lignin Activated Carbon is dissolved in zinc solution, addition iron salt solutions, surfactant reacts 0.5~2h, then 2~4h of mixing ultrasonic reaction is titrated using certain density aqueous slkali, control temperature that iron zinc-base Lignin Activated Carbon desulfurizing agent is obtained for 100~200 DEG C of 8~24h of reaction using autoclave, desulfurizing agent preparation technology flow is simple, desulfurized effect is good, iron zinc-base wood composite quality activated carbon improves the precision of active carbon desulfurization, can high temperature resistant.The lignin extracted using black liquid is original, truly realizes turning waste into wealth, with actual use value and social value.
Description
Technical field
The present invention relates to the preparation method of metal salt activated carbon, especially a kind of iron zinc-base wood composite quality activated carbon
The preparation method of desulfurizing agent.
Background technology
Current fume desulfurizing agent mainly has three kinds of modes：One is combustion desulfurization method, its method be added in coal it is a certain amount of
Sulphur-fixing agent, coal sulfur dioxide for generating in burning is reacted with sulphur-fixing agent, generation sulfate is discharged together with slag, this
Method is relatively costly；Another method is wet desulphurization, mainly using spray process, using two in alkaline aqueous solution absorption flue gas
Sulfur oxide, this method water consumption is big, and product is difficult after desulfurization, is also easy to produce secondary pollution, and cost of investment is high, and floor space is big
It is high with requirement for anticorrosion needed for equipment；Still an alternative is that active carbon adsorption, the usage cycles of the method activated carbon are shorter,
Regeneration is complex and desulfuration efficiency is low, and it is big to carry out washing water consumption, also easily causes secondary pollution, and activated carbon price compared with
It is high so that desulphurization cost increases.
The content of the invention
It is an object of the invention to provide a kind of SO that can effectively remove in waste gas2、SO3、H2S, organic sulfur etc., and
Desulfurization precision and the excellent iron zinc-base wood composite quality activated carbon desulphurization agent of resistance to elevated temperatures and preparation method thereof.
In order to realize above-mentioned technical purpose, the technical scheme is that：
A kind of iron zinc-base wood composite quality activated carbon desulphurization agent, it is made up of the component of following weight portion：
100~300 parts of Lignin Activated Carbon；
55~75 parts of zinc solution；
100~140 parts of iron salt solutions；
1~15 part of surfactant；
50~80 parts of aqueous slkali.
Further, described Lignin Activated Carbon is obtained by following component：
300~450 parts of masson pine black liquid；
50~80 parts of SPA.
Preferably, the solid content of the masson pine black liquid is 45%~60%.
Further, described zinc solution is in zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, zinc oxalate, zinc citrate
At least one mix.
Further, described iron salt solutions are at least in iron chloride, ferric nitrate, ferric sulfate, ironic citrate, ferric oxalate
Plant and mix.
Further, described surfactant is neopelex, cetyl trimethylammonium bromide, hexadecane
At least one in base trimethylammonium bromide, dodecyl sodium sulfate is mixed.
Further, described aqueous slkali be NaOH, at least one mixing in potassium hydroxide, ammoniacal liquor, limewash and
Into.
A kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent, it comprises the following steps：
S1. the preparation of Lignin Activated Carbon：Masson pine black liquid is weighed by metering, and adds SPA to be mixed, then will
After mixed solution system temperature adjustment carries out 8 ~ 16h of isothermal reaction to 55~90 DEG C, mixed solution is placed in tube furnace, makes to mix
After conjunction solution carries out 5 ~ 10h of calcining carbonization under the atmosphere of nitrogen with 400~800 DEG C of temperature, you can lignin activity is obtained
Charcoal；
S2. recombination reaction：Weigh Lignin Activated Carbon obtained above by metering and be dissolved in zinc solution, then again according to
Sequence is added iron salt solutions and surfactant and carries out 0.5~2h of hybrid reaction, after the completion of reaction, mixed solution is added into ultrasound
Ultrasonic mixing is carried out in wave device and reacts 2~4h, using aqueous slkali to the mixing in ultrasonic equipment during ultrasonic mixing
Solution is titrated, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：By product obtained in above-mentioned S2 be added in autoclave with
100~200 DEG C of temperature carries out 8~24h of reaction, after then product is leached and washed using absolute ethyl alcohol, then will wash
Product after washing is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 75~120 DEG C of temperature, you can be obtained
Iron zinc-base wood composite quality activated carbon desulphurization agent.
Further, the specific surface area of iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the step S3 be 540~
1243m2/g。
A kind of application of iron zinc-base wood composite quality activated carbon desulphurization agent, by described iron zinc-base wood composite quality activated carbon
Desulfurizing agent applies the SO in high temperature coal flue gas2Removing.
Using above-mentioned technical scheme, beneficial effects of the present invention are：
（1）Because the black liquid utilization rate produced in current paper-making process is less than 1%, the present invention program is black by using papermaking
Liquid wide material sources but also also a saving timber and bamboo charcoal resource as the carbon source for preparing Lignin Activated Carbon, not only, increased
On the premise of economic benefit, additionally it is possible to reach recycling using the effect with environmental protection；
（2）Using iron zinc-base wood composite quality activated carbon, desulfurization can be thoroughly carried out rapidly by alkaline metal cpds, and
And iron zinc-base wood composite quality activated carbon can be removed effectively the SO in waste gas as desulfurizing agent2、SO3、H2S, organic sulfur
Deng, and the desulfurization precision of activated carbon can be improved using iron zinc-base wood composite quality activated carbon and the high temperature resistant of activated carbon is improved
Performance.
Specific embodiment
A kind of iron zinc-base wood composite quality activated carbon desulphurization agent, it is made up of the component of following weight portion：
100~300 parts of Lignin Activated Carbon；
55~75 parts of zinc solution；
100~140 parts of iron salt solutions；
1~15 part of surfactant；
50~80 parts of aqueous slkali.
Further, described Lignin Activated Carbon is obtained by following component：
300~450 parts of masson pine black liquid；
50~80 parts of SPA.
Preferably, the solid content of the masson pine black liquid is 45%~60%.
Further, described zinc solution is in zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, zinc oxalate, zinc citrate
At least one mix.
Further, described iron salt solutions are at least in iron chloride, ferric nitrate, ferric sulfate, ironic citrate, ferric oxalate
Plant and mix.
Further, described surfactant is neopelex, cetyl trimethylammonium bromide, hexadecane
At least one in base trimethylammonium bromide, dodecyl sodium sulfate is mixed.
Further, described aqueous slkali be NaOH, at least one mixing in potassium hydroxide, ammoniacal liquor, limewash and
Into.
A kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent, it comprises the following steps：
S1. the preparation of Lignin Activated Carbon：Masson pine black liquid is weighed by metering, and adds SPA to be mixed, then will
After mixed solution system temperature adjustment carries out 8 ~ 16h of isothermal reaction to 55~90 DEG C, mixed solution is placed in tube furnace, makes to mix
After conjunction solution carries out 5 ~ 10h of calcining carbonization under the atmosphere of nitrogen with 400~800 DEG C of temperature, you can lignin activity is obtained
Charcoal；
S2. recombination reaction：Weigh Lignin Activated Carbon obtained above by metering and be dissolved in zinc solution, then again according to
Sequence is added iron salt solutions and surfactant and carries out 0.5~2h of hybrid reaction, after the completion of reaction, mixed solution is added into ultrasound
Ultrasonic mixing is carried out in wave device and reacts 2~4h, using aqueous slkali to the mixing in ultrasonic equipment during ultrasonic mixing
Solution is titrated, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：By product obtained in above-mentioned S2 be added in autoclave with
100~200 DEG C of temperature carries out 8~24h of reaction, after then product is leached and washed using absolute ethyl alcohol, then will wash
Product after washing is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 75~120 DEG C of temperature, you can be obtained
Iron zinc-base wood composite quality activated carbon desulphurization agent.
Further, the specific surface area of iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the step S3 be 540~
1243m2/g。
A kind of application of iron zinc-base wood composite quality activated carbon desulphurization agent, by described iron zinc-base wood composite quality activated carbon
Desulfurizing agent applies the SO in high temperature coal flue gas2Removing.
Embodiment 1
A kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent, it comprises the following steps：
S1. the preparation of Lignin Activated Carbon：The masson pine black liquid that 300 parts of solid contents are 45% is taken, by 6:1 rate of charge adds
Enter 50 parts of SPAs to be mixed, then after mixed solution system temperature adjustment is carried out into isothermal reaction 8h to 55 DEG C, will mix molten
Liquid is placed in tube furnace, after mixed solution is carried out calcining carbonization 5h with 400 DEG C of temperature under the atmosphere of nitrogen, you can be obtained
Lignin Activated Carbon；
S2. recombination reaction：Take 300 parts of Lignin Activated Carbons obtained above and be dissolved in 55 parts of zinc nitrate solutions, then
Sequentially adding 100 parts of iron nitrate solutions and 1 part of neopelex again carries out hybrid reaction 0.5h, after the completion of reaction, will
Mixed solution carries out ultrasonic mixing reaction 2h in being added to ultrasonic equipment, and 80 parts of NaOH are used during ultrasonic mixing
Mixed solution in ultrasonic equipment is titrated, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：It is anti-that intermediate product obtained in taking 104 parts of above-mentioned S2 is added to high pressure
Answer and reaction 8h is carried out with 100 DEG C of temperature in kettle, after then product is leached and washed using absolute ethyl alcohol, then will washing
Product afterwards is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 75 DEG C of temperature, you can iron zinc-base is obtained
Wood composite quality activated carbon desulphurization agent.
Performance test
Iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment is carried out into specific surface area detection, after testing gained
Specific surface area result is 790m2/g。
Bring iron zinc-base wood composite quality activated carbon desulphurization agent synthesis of air obtained in the present embodiment into quartz reactor
In, it is sufficiently mixed with simulated flue gas, wherein SO in simulated flue gas2Content be 1000ppm, use SO2Analyzer monitoring reactor goes out
SO in mouth flue gas2Changes of contents, final test obtains iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment
To SO2The adsorbable Sulfur capacity of institute is 340mg/g.
Embodiment 2
A kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent, it comprises the following steps：
S1. the preparation of Lignin Activated Carbon：The masson pine black liquid that 420 parts of solid contents are 60% is taken, by 7:1 rate of charge adds
Enter 60 parts of SPAs to be mixed, then after mixed solution system temperature adjustment is carried out into isothermal reaction 16h to 70 DEG C, will mix molten
Liquid is placed in tube furnace, after mixed solution is carried out calcining carbonization 10h with 600 DEG C of temperature under the atmosphere of nitrogen, you can system
Obtain Lignin Activated Carbon；
S2. recombination reaction：Take 200 parts of Lignin Activated Carbons obtained above and be dissolved in 60 parts of zinc acetate solutions, then
Sequentially adding 130 parts of oxalic acid ferrous solutions and 8 parts of cetyl trimethylammonium bromides again carries out hybrid reaction 1h, after the completion of reaction,
Mixed solution is added in ultrasonic equipment carries out ultrasonic mixing reaction 3h, uses 60 parts of ammoniacal liquor molten during ultrasonic mixing
Liquid is titrated to the mixed solution in ultrasonic equipment, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：It is anti-that intermediate product obtained in taking 62 parts of above-mentioned S2 is added to high pressure
Answer and reaction 16h is carried out with 150 DEG C of temperature in kettle, after then product is leached and washed using absolute ethyl alcohol, then will wash
Product after washing is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 100 DEG C of temperature, you can iron zinc is obtained
Base wood composite quality activated carbon desulphurization agent.
Performance test
Iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment is carried out into specific surface area detection, after testing gained
Specific surface area result is 1243m2/g。
Bring iron zinc-base wood composite quality activated carbon desulphurization agent synthesis of air obtained in the present embodiment into quartz reactor
In, it is sufficiently mixed with simulated flue gas, wherein SO in simulated flue gas2Content be 1000ppm, use SO2Analyzer monitoring reactor goes out
SO in mouth flue gas2Changes of contents, final test obtains iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment
To SO2The adsorbable Sulfur capacity of institute is 432mg/g.
Embodiment 3
A kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent, it comprises the following steps：
S1. the preparation of Lignin Activated Carbon：The masson pine black liquid that 450 parts of solid contents are 55% is taken, by 5.6:1 rate of charge
Add 80 parts of SPAs to be mixed, then after mixed solution system temperature adjustment is carried out into isothermal reaction 12h to 90 DEG C, will mix
Solution is placed in tube furnace, after mixed solution is carried out calcining carbonization 8h with 800 DEG C of temperature under the atmosphere of nitrogen, you can system
Obtain Lignin Activated Carbon；
S2. recombination reaction：Take 100 parts of Lignin Activated Carbons obtained above and be dissolved in 75 parts of solution of zinc sulfate, then
Sequentially adding 140 parts of ferrum sulfuricum oxydatum solutums and 15 parts of dodecyl sodium sulfates again carries out hybrid reaction 2h, after the completion of reaction, will mix
Solution carries out ultrasonic mixing reaction 4h in being added to ultrasonic equipment, and 50 parts of potassium hydroxide solutions are used during ultrasonic mixing
Mixed solution in ultrasonic equipment is titrated, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：It is anti-that intermediate product obtained in taking 190 parts of above-mentioned S2 is added to high pressure
Answer and reaction 24h is carried out with 200 DEG C of temperature in kettle, after then product is leached and washed using absolute ethyl alcohol, then will wash
Product after washing is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 120 DEG C of temperature, you can iron zinc is obtained
Base wood composite quality activated carbon desulphurization agent.
Performance test
Iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment is carried out into specific surface area detection, after testing gained ratio
Surface area result is 540m2/g。
Bring iron zinc-base wood composite quality activated carbon desulphurization agent synthesis of air obtained in the present embodiment into quartz reactor
In, it is sufficiently mixed with simulated flue gas, wherein SO in simulated flue gas2Content be 1000ppm, use SO2Analyzer monitoring reactor goes out
SO in mouth flue gas2Changes of contents, final test obtains iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the present embodiment
To SO2The adsorbable Sulfur capacity of institute is 269mg/g.
Wherein the zinc solution of above-described embodiment can also from zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, zinc oxalate,
At least one mixing in zinc citrate carries out replacement and uses；Iron salt solutions can also from iron chloride, ferric nitrate, ferric sulfate,
At least one mixing in ironic citrate, ferric oxalate carries out replacement and uses；Surfactant can also be DBSA
At least one in sodium, cetyl trimethylammonium bromide, cetyl trimethylammonium bromide, dodecyl sodium sulfate is mixed into
Row replacement is used；Aqueous slkali can be that at least one mixing in NaOH, potassium hydroxide, ammoniacal liquor, limewash is substituted
Use.
The foregoing is only of the invention for example, for a person skilled in the art, religion of the invention
Lead, without departing from the principles and spirit of the present invention all impartial changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to covering scope of the invention.
Claims (10)
1. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent, it is characterised in that：It is made up of the component of following weight portion：
100~300 parts of Lignin Activated Carbon；
55~75 parts of zinc solution；
100~140 parts of iron salt solutions；
1~15 part of surfactant；
50~80 parts of aqueous slkali.
2. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, it is characterised in that：Described wood
Quality activated carbon is obtained by following component：
300~450 parts of masson pine black liquid；
50~80 parts of SPA.
3. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 2, it is characterised in that：The horse hair
The solid content of loose black liquid is 45%~60%.
4. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, it is characterised in that：Described zinc
Salting liquid is that at least one in zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, zinc oxalate, zinc citrate is mixed.
5. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, it is characterised in that：Described iron
Salting liquid is that at least one in iron chloride, ferric nitrate, ferric sulfate, ironic citrate, ferric oxalate is mixed.
6. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, it is characterised in that：Described table
Face activating agent is neopelex, cetyl trimethylammonium bromide, cetyl trimethylammonium bromide, dodecyl
At least one in sodium sulfonate is mixed.
7. a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, it is characterised in that：Described alkali
Solution is that at least one in NaOH, potassium hydroxide, ammoniacal liquor, limewash is mixed.
8. a kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 1, its feature exists
In：It comprises the following steps：
S1. the preparation of Lignin Activated Carbon：Masson pine black liquid is weighed by metering, and adds SPA to be mixed, then will
After mixed solution system temperature adjustment carries out 8 ~ 16h of isothermal reaction to 55~90 DEG C, mixed solution is placed in tube furnace, makes to mix
After conjunction solution carries out 5 ~ 10h of calcining carbonization under the atmosphere of nitrogen with 400~800 DEG C of temperature, you can lignin activity is obtained
Charcoal；
S2. recombination reaction：Weigh Lignin Activated Carbon obtained above by metering and be dissolved in zinc solution, then again according to
Sequence is added iron salt solutions and surfactant and carries out 0.5~2h of hybrid reaction, after the completion of reaction, mixed solution is added into ultrasound
Ultrasonic mixing is carried out in wave device and reacts 2~4h, using aqueous slkali to the mixing in ultrasonic equipment during ultrasonic mixing
Solution is titrated, after ultrasonic mixing reaction terminates, you can intermediate product is obtained；
S3. iron zinc-base Lignin Activated Carbon hydrothermal synthesis reaction：Intermediate product obtained in above-mentioned S2 is added to autoclave
In 8~24h of reaction is carried out with 100~200 DEG C of temperature, after then product is leached and washed using absolute ethyl alcohol, then
Product after washing is placed in Minton dryer, carries out being dried under vacuum to product constant weight with 75~120 DEG C of temperature, you can
Iron zinc-base wood composite quality activated carbon desulphurization agent is obtained.
9. a kind of preparation method of iron zinc-base wood composite quality activated carbon desulphurization agent according to claim 8, its feature exists
In：The specific surface area of iron zinc-base wood composite quality activated carbon desulphurization agent obtained in the step S3 is 540~1243m2/g。
10. the application of a kind of iron zinc-base wood composite quality activated carbon desulphurization agent according to any of the above-described claim, it is special
Levy and be：Described iron zinc-base wood composite quality activated carbon desulphurization agent is applied into the SO in high temperature coal flue gas2Removing.
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