CN109173978A - A kind of preparation method of N doping hydrotalcite adsorbent - Google Patents
A kind of preparation method of N doping hydrotalcite adsorbent Download PDFInfo
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- CN109173978A CN109173978A CN201811091381.3A CN201811091381A CN109173978A CN 109173978 A CN109173978 A CN 109173978A CN 201811091381 A CN201811091381 A CN 201811091381A CN 109173978 A CN109173978 A CN 109173978A
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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Abstract
The invention discloses a kind of preparation methods of N doping hydrotalcite adsorbent.The N doping hydrotalcite adsorbent the preparation method comprises the following steps: by double drop coprecipitations, prepare calcium and magnesium aluminum hydrotalcite, the mixing salt solution of different proportion and aqueous slkali mixed, be aged, washing obtains calcium and magnesium aluminum hydrotalcite after dry；It is mixed in a certain ratio and grinds with urea, melamine, hexa one of which as nitrogen source using calcium and magnesium aluminum hydrotalcite as presoma, obtained sample is calcined in nitrogen atmosphere, the N doping hydrotalcite adsorbent is made.The houghite adsorbent of N doping prepared by the present invention is having good adsorption effect, high temperature resistant to sour gas such as hydrogen chloride gas, and large amount of adsorption is a kind of high-performance adsorbent for acid gas removals such as hydrogen chloride.
Description
Technical field
The present invention relates to hydrotalcite adsorbents, and in particular to a kind of preparation method of N doping hydrotalcite adsorbent.
Background technique
Hydrogen chloride (HCl) gas in flue gas causes very big harm to boiler, not only causes superheater in boiler system
The low-temperature corrosion of high temperature corrosion, back-end surfaces with reheater, can also damage detection instrument, improve the operation and maintenance of equipment
Cost.HCl, which is discharged into after atmosphere, can also destroy ozone layer, cause the environmental problems such as photochemical fog and acid rain.
Hydrotalcite-like materials and its product of roasting are mainly employed as new catalyst or are urged in terms of catalysis
Agent carrier has preferable utilization in the organic reactions such as catalytic hydrogenation, alcohols conversion, cracking, polycondensation.It is being used as catalyst side
Due to may serve as base catalyst there are alkali center in face, hydrotalcite-like materials and its product of roasting, in many reactions
In, the catalytic effect of hydrotalcite-like materials is better than traditional catalyst material (such as sodium hydroxide, potassium hydroxide).Houghite
Material has wide application in the catalysis reaction such as dehydrogenation plus hydrogen and cracking reformation at present.And hydrotalcite-like materials compare biography
System catalyst, there is high catalytic activity, high stability.Hydrotalcite-like materials are because have interlayer ion interchangeability, knot
Structure memory effect, these alkaline characteristics, are widely used in removing NOx、HCl、SO2、CO2Harmful sour gas in equal atmosphere.
The calcium magnesia-alumina hydrotalcite synthesized using the characteristics of hydrotalcite layered structure shows good removing HCl
Can, and this adsorbent can be synthesized in laboratory conditions.But usually there is alkaline fast, the high temperature item that fails in this adsorbent
Meltable warm slagging, product are having the defects of H, be not sufficiently stable in the existing high-temperature atmosphere of O under part, cause adsorbance inadequate
Greatly, adsorption efficiency is not high, influences dechlorination effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of N doping hydrotalcite adsorbent, and it is raw to solve burning power plant
The content of acid gas such as hydrogen chloride in tail gas are high during production, the not high technical problem of dechlorination efficiency.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention:
A kind of preparation method of N doping hydrotalcite adsorbent, includes the following steps:
Step 1) prepares calcium and magnesium aluminum hydrotalcite by double drop coprecipitations；With solvable magnesium salts, solvable aluminium salt, soluble calcium salt
Mixing salt solution is prepared, calcium and magnesium al mole ratio range is 1~3: 1~3: 1 in mixing salt solution；With sodium carbonate or sodium bicarbonate and
The mixed aqueous solution of sodium hydroxide is lye, under 65 degrees Celsius, respectively mixes salting liquid and aqueous slkali using double drop methods, adjusts
Integral drip speed, control pH range are 10~11, are aged 48h, wash drying, obtain calcium and magnesium aluminum hydrotalcite；
Step 2), the calcium and magnesium aluminum hydrotalcite obtained using step 1) is presoma, with urea, melamine or hexa-methylene four
One of amine is mixed with certain proportion, prepares the adsorbent of N doping hydrotalcite；By mixed hydrotalcite precursor
It is put into quartzy porcelain boat with nitrogen source, is roasted in nitrogen atmosphere using tube furnace, using room temperature as initial temperature, heating rate 5
Centigrade per minute is warming up to 650 degrees Celsius, is kept for 180 minutes；The suction of N doping hydrotalcite is obtained after secondary high-temperature roasts again
Attached dose.
Preferably, soluble calcium salt described in step 1), solvable magnesium salts, soluble aluminum salt are respectively calcium nitrate, magnesium nitrate, nitre
Sour aluminium, the aqueous slkali are the mixed aqueous solution of the sodium carbonate that concentration is 1mol/L and the sodium hydroxide of 1.5mol/L.
As a preferred embodiment 1, calcium and magnesium al mole ratio is 1.5: 1.5: 1 in the step 1) salting liquid, and step 2) is described
Calcium and magnesium aluminum hydrotalcite and urea quality ratio are 1: 1.
As a preferred embodiment 2, calcium and magnesium al mole ratio is 1.7: 1.7: 1 in the step 1) salting liquid, and step 2) is described
Calcium and magnesium aluminum hydrotalcite and urea quality ratio are 2: 1.
As a preferred embodiment 3, calcium and magnesium al mole ratio is 2: 2: 1 in the step 1) salting liquid, the step 2) calcium and magnesium
Aluminum hydrotalcite and urea quality ratio are 2: 1.
As a preferred embodiment 4, calcium and magnesium al mole ratio is 2: 2: 1 in the step 1) salting liquid, the step 2) calcium and magnesium
Aluminum hydrotalcite and hexa mass ratio are 2: 1.
As a preferred embodiment 5, calcium and magnesium al mole ratio is 2: 2: 1 in the step 1) salting liquid, the step 2) calcium and magnesium
Aluminum hydrotalcite and melamine mass ratio are 2: 1.
Preferably, the temperature of the roasting of secondary high-temperature described in step 2) is 700 degrees Celsius, calcining time 8h.
Nitrogen source is introduced in adsorbent, it is possible to increase the specific surface area and pore volume of adsorbent, and show adsorbent
Better high temperature resistant and anti-caking power, so that the dechlorination of adsorbent is further increased, the sour gas such as especially HCl.
Before the study found that the calcium and magnesium aluminum hydrotalcite of laboratory synthesis has good alkalinity for HCl gas removal, but exist easy
Sintering, mechanical strength is inadequate, reaches the problems such as adsorption saturation state for time is short.So introducing urea, melamine, hexa-methylene
These three common nitrogen sources of tetramine, using the different number nitrogen-atoms institutes having electronic number of its band, the hydrogen in easily capture HCl is former
Son reaches higher removal effect to reduce the generation of HCl.
Compared with prior art, the invention has the following beneficial effects:
A kind of adsorbent of N doping hydrotalcite produced by the present invention carries out dechlorination test under certain reaction condition,
It undopes than originally and shows better dechlorination effect, dechlorination efficiency reaches 99.9%, and increases specific surface area and hole
Rate, to increase the duration of absorption so as to adsorb the HCl gas of more volumes.Meanwhile N doping provides for adsorbent
Nitrogen functional group abundant, reduces the size of adsorbent, it is excellent can be prepared into raising mechanical strength of some fixed shapes etc.
Point.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail below by way of specific embodiment.Raw materials and reagents used in the present invention
It is commercially available.
Specific embodiment 1:
In the present embodiment 1, calcium and magnesium al mole ratio is 1.5: 1.5: 1 in salting liquid.
61.53g magnesium nitrate, 60.02g aluminum nitrate, 58.18g calcium nitrate are made into salting liquid, are by concentration by step 1)
It is aqueous slkali that the mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L, which is matched,.Under 65 degrees Celsius, using double
Drop method mixes salting liquid and aqueous slkali, and adjustment drop speed, control pH range is 10~11, is aged 48h, washs drying, obtain
Calcium and magnesium aluminum hydrotalcite；Being subsequently placed in drying in 150 DEG C of baking ovens, for 24 hours, the sample after drying saves backup.
Step 2) is mixed using the calcium and magnesium aluminum hydrotalcite of above-mentioned acquisition as presoma with urea with the ratio of mass ratio 1: 1
It closes, is put into quartzy porcelain boat, is roasted in nitrogen atmosphere using tube furnace, using room temperature as initial temperature, heating rate is 5 Celsius
Degree per minute, is warming up to 650 degrees Celsius, keeps 180min.Product after drying is roasted into 8h under 700 degrees Celsius, obtains one
Kind N doping hydrotalcite adsorbent 1.
2g adsorbent 1 described above is weighed, HCl fixed bed of sorbent performance testing device is put into, removal efficiency reaches
75.7%, the adsorbent out-of-service time is 65min.
Specific embodiment 2:
In the present embodiment 2, calcium and magnesium al mole ratio is 1.7: 1.7: 1 in salting liquid.
69.75g magnesium nitrate, 60.02g aluminum nitrate, 65.94g calcium nitrate are made into salting liquid, are by concentration by step 1)
It is aqueous slkali that the mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L, which is matched,.Under 65 degrees Celsius, using double
It drips coprecipitation respectively to mix salting liquid and aqueous slkali, adjustment drop speed, control pH range is 10~11, is aged 48h, washing
It is dry, obtain magnesium-aluminum-calcium hydrotalcite；Being subsequently placed in drying in 150 DEG C of baking ovens, for 24 hours, the sample after drying saves backup.
Step 2) is mixed using the calcium and magnesium aluminum hydrotalcite of above-mentioned acquisition as presoma with urea with the ratio of mass ratio 2: 1
It closes, is put into quartzy porcelain boat, is roasted in nitrogen atmosphere using tube furnace, using room temperature as initial temperature, heating rate is 5 Celsius
Degree per minute, is warming up to 650 degrees Celsius, keeps 180min.Product after drying is roasted into 8h under 700 degrees Celsius, obtains one
The adsorbent 2 of kind N doping hydrotalcite.
2g adsorbent 2 described above is weighed, HCl performance of the adsorbent test device is put into, removal efficiency reaches 84.5%, inhales
Attached dose of out-of-service time is 98min.
Specific embodiment 3:
In the present embodiment 3, calcium and magnesium al mole ratio is 2: 2: 1 in salting liquid.
82.05g magnesium nitrate, 60.02g aluminum nitrate, 77.57g calcium nitrate are made into salting liquid, are by concentration by step 1)
It is aqueous slkali that the mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L, which is matched, under 65 degrees Celsius, using double
It dripping coprecipitation respectively to mix the mixing salt solution of different proportion and aqueous slkali, adjustment drop speed, control pH range is 10~
11, it is aged 48h, drying is washed, obtains calcium and magnesium aluminum hydrotalcite；It is subsequently placed in 150 DEG C of baking ovens and dries for 24 hours, the sample after drying
It saves backup.
Step 2) is mixed using the calcium and magnesium aluminum hydrotalcite of above-mentioned acquisition as presoma with urea with the ratio of mass ratio 2: 1
It closes, is put into quartzy porcelain boat, is roasted in atmosphere using tube furnace, using room temperature as initial temperature, heating rate is 5 degrees Celsius every
Minute, 650 degrees Celsius are warming up to, 180min is kept.Product after drying is roasted into 8h under 700 degrees Celsius, obtains a kind of nitrogen
Adulterate the adsorbent 3 of hydrotalcite.
2g adsorbent 3 as described above is weighed, HCl performance of the adsorbent test device is put into, removal efficiency reaches 90.1%, inhales
Attached dose of out-of-service time is 147min.
Specific embodiment 4:
In the present embodiment 4, calcium and magnesium al mole ratio is 2: 2: 1 in salting liquid.
82.05g magnesium nitrate, 60.02g aluminum nitrate, 77.57g calcium nitrate are made into salting liquid, are by concentration by step 1)
It is aqueous slkali that the mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L, which is matched, under 65 degrees Celsius, using double
It dripping coprecipitation respectively to mix the mixing salt solution of different proportion and aqueous slkali, adjustment drop speed, control pH range is 10~
11, it is aged 48h, drying is washed, obtains calcium and magnesium aluminum hydrotalcite；It is subsequently placed in 150 DEG C of baking ovens and dries for 24 hours, the sample after drying
It saves backup.
Step 2), using the calcium and magnesium aluminum hydrotalcite of above-mentioned acquisition as presoma, and hexa is with the ratio of mass ratio 2:1
Example is mixed, and is put into quartzy porcelain boat, is roasted in atmosphere using tube furnace, using room temperature as initial temperature, heating rate 5
Centigrade per minute is warming up to 650 degrees Celsius, keeps 180min.Product after drying is roasted into 8h under 700 degrees Celsius, is obtained
To a kind of adsorbent 4 of N doping hydrotalcite.2g adsorbent 4 is weighed, HCl performance of the adsorbent test device, removal efficiency are put into
Reach 94.7%, the adsorbent out-of-service time is 185min.
Specific embodiment 5:
In the present embodiment 5, calcium and magnesium al mole ratio is 2: 2: 1 in salting liquid.
82.05g magnesium nitrate, 60.02g aluminum nitrate, 77.57g calcium nitrate are made into salting liquid, are by concentration by step 1)
It is aqueous slkali that the mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L, which is matched, under 65 degrees Celsius, using double
It dripping coprecipitation respectively to mix the mixing salt solution of different proportion and aqueous slkali, adjustment drop speed, control pH range is 10~
11, it is aged 48h, drying is washed, obtains calcium and magnesium aluminum hydrotalcite；It is subsequently placed in 150 DEG C of baking ovens and dries for 24 hours, the sample after drying
It saves backup.
Step 2), using the calcium and magnesium aluminum hydrotalcite of above-mentioned acquisition as presoma, with melamine with the ratio of mass ratio 2:1 into
Row mixing, is put into quartzy porcelain boat, is roasted in atmosphere using tube furnace, and using room temperature as initial temperature, heating rate is 5 Celsius
Degree per minute, is warming up to 650 degrees Celsius, keeps 180min.Product after drying is roasted into 8h under 700 degrees Celsius, obtains one
The adsorbent 5 of kind N doping hydrotalcite.
2g adsorbent 5 as described above is weighed, HCl performance of the adsorbent test device is put into, removal efficiency reaches 98.8%, inhales
Attached dose of out-of-service time is 221min.
Comparative example 1-5, it was demonstrated that a kind of preparation method of the adsorbent for the N doping hydrotalcite that this patent proposes is
Feasible, the adsorbent of different types of nitrogen source doping hydrotalcite can effectively realize dechlorination effect.It finds simultaneously, by calcium and magnesium aluminium
Calcium molar ratio is that 2: 2: 1 to prepare hydrotalcites most suitable as presoma, in three kinds of nitrogen sources, nitrogen function that melamine contains because of it
Group is most, so that the N doping hydrotalcite of synthesis is all optimal in the amount and efficiency of removing HCl gas.
Claims (8)
1. a kind of preparation method of N doping hydrotalcite adsorbent, which comprises the steps of:
Step 1) prepares calcium and magnesium aluminum hydrotalcite by double drop coprecipitations；It is prepared with solvable magnesium salts, solvable aluminium salt, soluble calcium salt
Mixing salt solution, calcium and magnesium al mole ratio range is 1~3: 1~3: 1 in mixing salt solution；
Using the mixed aqueous solution of sodium carbonate or sodium bicarbonate and sodium hydroxide as lye, under 65 degrees Celsius, using double drop methods point
Salting liquid and aqueous slkali are not mixed, adjustment drop speed, control pH range is 10~11, is aged 48h, washs drying, obtain calcium
Magnalium hydrotalcite；
Step 2), the calcium and magnesium aluminum hydrotalcite obtained using step 1) is presoma, in urea, melamine or hexa
One kind mixed with certain proportion, prepare the adsorbent of N doping hydrotalcite；By mixed hydrotalcite precursor and nitrogen
Source is put into quartzy porcelain boat, is roasted in nitrogen atmosphere using tube furnace, and using room temperature as initial temperature, heating rate is 5 Celsius
Degree per minute, is warming up to 650 degrees Celsius, is kept for 180 minutes；The absorption of N doping hydrotalcite is obtained after secondary high-temperature roasts again
Agent.
2. the preparation method of N doping hydrotalcite adsorbent according to claim 1, which is characterized in that described in step 1)
Soluble calcium salt, solvable magnesium salts, soluble aluminum salt be respectively calcium nitrate, magnesium nitrate, aluminum nitrate, the aqueous slkali is that concentration is
The mixed aqueous solution of the sodium hydroxide of the sodium carbonate and 1.5mol/L of 1mol/L.
3. the preparation method of N doping hydrotalcite adsorbent according to claim 1 or 2, which is characterized in that step 1) institute
Stating calcium and magnesium al mole ratio in salting liquid is 1.5: 1.5: 1, and step 2) the calcium and magnesium aluminum hydrotalcite and urea quality ratio are 1: 1.
4. the preparation method of N doping hydrotalcite adsorbent according to claim 1 or 2, which is characterized in that step 1) institute
Stating calcium and magnesium al mole ratio in salting liquid is 1.7: 1.7: 1, and step 2) the calcium and magnesium aluminum hydrotalcite and urea quality ratio are 2: 1.
5. the preparation method of N doping hydrotalcite adsorbent according to claim 1 or 2, which is characterized in that step 1) institute
Stating calcium and magnesium al mole ratio in salting liquid is 2: 2: 1, and step 2) the calcium and magnesium aluminum hydrotalcite and urea quality ratio are 2: 1.
6. the preparation method of N doping hydrotalcite adsorbent according to claim 1 or 2, which is characterized in that step 1) institute
Stating calcium and magnesium al mole ratio in salting liquid is 2: 2: 1, and step 2) the calcium and magnesium aluminum hydrotalcite and hexa mass ratio are 2:
1。
7. the preparation method of N doping hydrotalcite adsorbent according to claim 1 or 2, which is characterized in that step 1) institute
Stating calcium and magnesium al mole ratio in salting liquid is 2: 2: 1, and step 2) the calcium and magnesium aluminum hydrotalcite and melamine mass ratio are 2: 1.
8. the preparation method of N doping hydrotalcite adsorbent according to claim 1, which is characterized in that described in step 2)
The temperature of secondary high-temperature roasting is 700 degrees Celsius, calcining time 8h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624529A (en) * | 2019-09-26 | 2019-12-31 | 中国天辰工程有限公司 | Preparation and use methods of hydroxide intercalation calcium magnesium aluminum hydrotalcite solid base catalyst |
| CN111217385A (en) * | 2020-02-23 | 2020-06-02 | 武汉工程大学 | Method for preparing calcium-magnesium-aluminum hydrotalcite by using phosphate tailings |
| CN111410175A (en) * | 2020-03-10 | 2020-07-14 | 上海大学 | N-doped modified L DHs material and preparation method thereof |
| CN112090439A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院大学 | Nitrogen-doped hydrotalcite-like derivative composite oxide material and preparation method and application thereof in low-temperature carbonyl sulfide hydrolysis reaction |
| CN112517039A (en) * | 2020-12-09 | 2021-03-19 | 万华化学集团股份有限公司 | Novel nitrogen modified composite metal oxide insertion type catalyst and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624529A (en) * | 2019-09-26 | 2019-12-31 | 中国天辰工程有限公司 | Preparation and use methods of hydroxide intercalation calcium magnesium aluminum hydrotalcite solid base catalyst |
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| CN111410175A (en) * | 2020-03-10 | 2020-07-14 | 上海大学 | N-doped modified L DHs material and preparation method thereof |
| CN112090439A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院大学 | Nitrogen-doped hydrotalcite-like derivative composite oxide material and preparation method and application thereof in low-temperature carbonyl sulfide hydrolysis reaction |
| CN112090439B (en) * | 2020-09-18 | 2023-02-21 | 中国科学院大学 | Nitrogen-doped hydrotalcite-like derivative composite oxide material and preparation method and application thereof in low-temperature carbonyl sulfide hydrolysis reaction |
| CN112517039A (en) * | 2020-12-09 | 2021-03-19 | 万华化学集团股份有限公司 | Novel nitrogen modified composite metal oxide insertion type catalyst and application thereof |
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