CN109289806A - The preparation method of spherical formaldehyde adsorbent - Google Patents
The preparation method of spherical formaldehyde adsorbent Download PDFInfo
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- CN109289806A CN109289806A CN201811240947.4A CN201811240947A CN109289806A CN 109289806 A CN109289806 A CN 109289806A CN 201811240947 A CN201811240947 A CN 201811240947A CN 109289806 A CN109289806 A CN 109289806A
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- preparation
- spherical
- adsorption material
- methyl aldehyde
- aldehyde adsorption
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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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
- B01D53/02—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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
Abstract
The invention discloses a kind of preparation methods of spherical methyl aldehyde adsorption material, and based on resin-oatmeal, alcohols material and nitrogenous reagent are that object successively through dissolution, polymerization, solidification, charing and steam activation obtains spherical methyl aldehyde adsorption material.Raw material sources of the present invention are extensive, simple process is controllable, operating condition is mild, and removal efficiency of the gained spherical shape methyl aldehyde adsorption material under various concentration is up to 85% or more.
Description
Technical field
The invention belongs to the preparation technical field of methyl aldehyde adsorption material, specially a kind of preparation of spherical methyl aldehyde adsorption material
Method.
Background technique
In recent years, the environmental pollution that formaldehyde generates causes extensive concern, and active carbon adsorption is for removal formaldehyde
It is most effective, be primarily due to the more hollow structures of active carbon and determine that adsorption capacity is strong, and it is at low cost, effect is good, become absorption
The hot spot of Material Field research.The absorbent charcoal material reported at present is mostly particle or powdery, generally existing poor fluidity, adsorption energy
Power is poor, removes the disadvantages of formaldehyde low efficiency.
Substance containing amino can occur polycondensation reaction with the formaldehyde of absorption, effectively take off because it is with stronger activity
Except formaldehyde, the chemical property of adsorbent material is improved.It therefore, is raw material by using nitrogen substance on existing Research foundation
Spherical Carbon Materials are prepared, enhances mobility, while forming amino functional group in Carbon Materials structure by heat treatment process, changes
It is apt to its chemical adsorption capacity, forms efficient formaldehyde adsorbent material.
Summary of the invention
That it is an object of the present invention to provide a kind of simple processes is controllable, operating condition is mild, the good method preparation of removal performance
Spherical methyl aldehyde adsorption material.
The present invention is achieved by the following technical scheme:
A kind of preparation method of spherical shape methyl aldehyde adsorption material, comprising the following steps:
(1), resin-oatmeal and alcohols material are added in three-necked flask according to mass ratio 15 ~ 30:30 ~ 60, then add 10 ~
Then 30g polyvinyl alcohol stirs 1 ~ 2h in 70 DEG C of constant temperature；
(2), 20 ~ 40g nitrogenous reagent is added in above-mentioned solution, then stirs 6h in 95 DEG C of constant temperature；
(3), above-mentioned solution is filtered and transferred in evaporating dish, is statically placed in 180 DEG C of solidification 12h in vacuum drying oven, obtains
Resin balls；
(4), step (3) resulting resin balls are risen into 550 ~ 700 DEG C of 2 ~ 5h of charing by room temperature in high temperature process furnances, then will
Temperature rises to 800 ~ 950 DEG C, is passed through 50 ~ 120mL/min, 2 ~ 4h of steam activation, is naturally cooling to room temperature and obtains spherical formaldehyde suction
Enclosure material；
In above-mentioned preparation method, the resin-oatmeal is phenolic resin or Lauxite.
In above-mentioned preparation method, the alcohols is ethyl alcohol or ethylene glycol.
In above-mentioned preparation method, nitrogenous reagent described in step (2) is polyaniline or polyimides.
Beneficial effects of the present invention are as follows:
For the present invention based on resin-oatmeal, alcohols material and nitrogenous reagent are object, successively through dissolution, polymerization, solidification, charing and
Steam activation obtains spherical methyl aldehyde adsorption material.Raw material sources of the present invention are extensive, simple process is controllable, operating condition is mild,
Removal efficiency of the gained spherical shape methyl aldehyde adsorption material under various concentration is up to 85% or more.
The present invention has rational design, specific practical application and promotional value well.
Detailed description of the invention
Fig. 1 shows the SEM figures of spherical methyl aldehyde adsorption material prepared by embodiment 1.
Fig. 2 indicates the SEM figure of spherical methyl aldehyde adsorption material prepared by embodiment 2.
Fig. 3 indicates the SEM figure of spherical methyl aldehyde adsorption material prepared by embodiment 3.
Fig. 4 indicates the removing formaldehyde application under 4 various concentration of embodiment and the removing curve under comparative example 1,2 various concentrations
Figure.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
The preparation method of spherical shape methyl aldehyde adsorption material of the present invention, based on resin-oatmeal, alcohols material and nitrogenous
Reagent is object, successively through dissolution, polymerization, solidification, charing and steam activation, obtains spherical methyl aldehyde adsorption material.The present invention
Raw material sources are extensive, simple process is controllable, operating condition is mild, removing of the gained spherical shape methyl aldehyde adsorption material under various concentration
Rate is up to 85% or more.
Specific embodiment is as follows:
Embodiment 1
A kind of preparation method of spherical shape formaldehyde adsorbent, includes the following steps:
(1), 30g phenol-formaldehyde resin powder and 30g ethyl alcohol are added in three-necked flask, 10g polyvinyl alcohol are then added, then 70
DEG C constant temperature stirs 1h；
(2), 20g polyaniline is added in above-mentioned solution, then stirs 6h in 95 DEG C of constant temperature；
(3), above-mentioned solution is filtered and transferred in evaporating dish, is statically placed in 180 DEG C of solidification 12h in vacuum drying oven, obtains
Resin balls；
(4), above-mentioned resulting resin balls are risen into 550 DEG C of charing 5h by room temperature in high temperature process furnances, then rises to temperature
950 DEG C, it is passed through 50mL/min steam activation 2h, room temperature is naturally cooling to and obtains spherical methyl aldehyde adsorption material；
Fig. 1 shows the SEM figure of the spherical methyl aldehyde adsorption material of richness of the preparation of embodiment 1.
Embodiment 2
A kind of preparation method of spherical shape formaldehyde adsorbent, includes the following steps:
(1), 45g phenol-formaldehyde resin powder and 90g ethyl alcohol are added in three-necked flask, 20g polyvinyl alcohol are then added, then 70
DEG C constant temperature stirs 1.5h；
(2), 30g polyimides is added in above-mentioned solution, then stirs 4h in 95 DEG C of constant temperature；
(3), above-mentioned solution is filtered and transferred in evaporating dish, is statically placed in 180 DEG C of solidification 12h in vacuum drying oven, obtains
Resin balls；
(4), above-mentioned resulting resin balls are risen into 650 DEG C of charing 3.5h by room temperature in high temperature process furnances, then by temperature liter
To 870 DEG C, it is passed through 80mL/min steam activation 3h, room temperature is naturally cooling to and obtains spherical methyl aldehyde adsorption material；
Fig. 2 shows the SEM figures of spherical methyl aldehyde adsorption material prepared by embodiment 2.
Embodiment 3
A kind of preparation method of spherical shape formaldehyde adsorbent, includes the following steps:
(1), 90g phenol-formaldehyde resin powder and 120g ethyl alcohol are added in three-necked flask, then add 30g polyvinyl alcohol, then exists
70 DEG C of constant temperature stir 2h；
(2), 40g polyaniline is added in above-mentioned solution, then stirs 4h in 95 DEG C of constant temperature；
(3), above-mentioned solution is filtered and transferred in evaporating dish, is statically placed in 180 DEG C of solidification 12h in vacuum drying oven, obtains
Resin balls；
(4), above-mentioned resulting resin balls are risen into 700 DEG C of charing 2h by room temperature in high temperature process furnances, then rises to temperature
800 DEG C, it is passed through 120mL/min steam activation 4h, room temperature is naturally cooling to and obtains spherical methyl aldehyde adsorption material；
Fig. 3 shows the SEM figure of the spherical methyl aldehyde adsorption material of the preparation of embodiment 3.
The spherical methyl aldehyde adsorption material of 1,2,3 preparations through the embodiment of the present invention, it is obtained it can be seen from Fig. 1,2,3
Spherical methyl aldehyde adsorption material hole is flourishing.
Embodiment 4
The spherical methyl aldehyde adsorption material of 1,2,3 preparations tests the methanal removing under various concentration respectively through the embodiment of the present invention
Energy.
Specific experiment condition is: 30mg spherical shape methyl aldehyde adsorption material, and reacting in internal diameter is the atmospheric fixed bed anti-of 10mm
It answers and is carried out on device.Experiment simulation gas composition are as follows: the concentration of formaldehyde is 30-250mg/m3, N2For carrier gas, operation temperature is 25 DEG C,
Gas flow 1000mL/min, air speed 20000h-1.Exit concentration is carried out with gas chromatographicanalyzer (Agilent 7820A)
On-line real-time measuremen.
Comparative example 1
Using the methanal removing performance being not added in embodiment 1 under the adsorbent material test various concentration that polyaniline obtains, specifically
Experiment condition it is consistent with the experiment condition in embodiment 4.
Comparative example 2
Using the methanal removing performance being not added in embodiment 2 under the adsorbent material test various concentration that polyimides obtains, tool
The experiment condition of body is consistent with the experiment condition in embodiment 4.
Sample 1,2,3 and comparative example 1,2 methanal removing energy are measured respectively by on-line real-time measuremen, specifically such as Fig. 4 institute
Show, directly adopt embodiment 1 and embodiment 2 be not added with the methanal removing efficiency of the adsorbent material that nitrogenous reagent activates compared with
It is low, and pass through the removal efficiency of spherical methyl aldehyde adsorption material prepared by embodiment 1,2,3 up to 85% or more.
It should be pointed out that for the those skilled in the art of the art, without departing from the principle of the present invention,
Several improvement and application can also be made, these are improved and application is also considered as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of spherical shape formaldehyde adsorbent, characterized by the following steps:
(1), resin-oatmeal and alcohols material are added in three-necked flask according to mass ratio 15 ~ 30:30 ~ 60, then add 10 ~
Then 30g polyvinyl alcohol stirs 1 ~ 2h in 70 DEG C of constant temperature；
(2), 20 ~ 40g nitrogenous reagent is added in above-mentioned solution, then stirs 6h in 95 DEG C of constant temperature；
(3), above-mentioned solution is filtered and transferred in evaporating dish, is statically placed in 180 DEG C of solidification 12h in vacuum drying oven, obtains
Resin balls；
(4), step (3) resulting resin balls are risen into 550 ~ 700 DEG C of 2 ~ 5h of charing by room temperature in high temperature process furnances, then will
Temperature rises to 800 ~ 950 DEG C, is passed through 50 ~ 120mL/min, 2 ~ 4h of steam activation, is naturally cooling to room temperature and obtains spherical formaldehyde suction
Enclosure material.
2. the preparation method of spherical shape methyl aldehyde adsorption material according to claim 1, it is characterised in that: the resin-oatmeal is phenol
Urea formaldehyde or Lauxite.
3. the preparation method of spherical shape methyl aldehyde adsorption material according to claim 1, it is characterised in that: the alcohols is ethyl alcohol
Or ethylene glycol.
4. the preparation method of spherical shape methyl aldehyde adsorption material according to claim 1, it is characterised in that: described in step (2)
Nitrogenous reagent is polyaniline or polyimides.
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| CN201811240947.4A CN109289806B (en) | 2018-10-24 | 2018-10-24 | Preparation method of spherical formaldehyde adsorbent |
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| CN201811240947.4A CN109289806B (en) | 2018-10-24 | 2018-10-24 | Preparation method of spherical formaldehyde adsorbent |
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| CN109289806A true CN109289806A (en) | 2019-02-01 |
| CN109289806B CN109289806B (en) | 2021-04-06 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6013549A (en) * | 1983-07-01 | 1985-01-24 | 松下電工株式会社 | Method of impregnating base material with varnish |
| CN1303734A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Fibrous carbon-based catalytic adsorption material and its preparation method |
| US20060257770A1 (en) * | 2005-05-10 | 2006-11-16 | Xerox Corporation | Photoreceptors |
| CN104743543A (en) * | 2015-03-04 | 2015-07-01 | 同济大学 | Method for preparing polyaniline/phenolic aldehyde based carbon material |
| CN105895380A (en) * | 2016-04-12 | 2016-08-24 | 齐鲁工业大学 | Three-dimensional reticular polyaniline/phenolic resin-based carbon sphere composite material and preparation method thereof |
| CN107032320A (en) * | 2017-04-29 | 2017-08-11 | 成都博美实润科技有限公司 | A kind of preparation method based on polyaniline-modified phenolic resin base porous carbon |
| CN109289763A (en) * | 2018-10-24 | 2019-02-01 | 南京海洛阿姆生物科技有限公司 | A kind of cleanser and production technology removing formaldehyde in indoor air |
-
2018
- 2018-10-24 CN CN201811240947.4A patent/CN109289806B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6013549A (en) * | 1983-07-01 | 1985-01-24 | 松下電工株式会社 | Method of impregnating base material with varnish |
| CN1303734A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Fibrous carbon-based catalytic adsorption material and its preparation method |
| US20060257770A1 (en) * | 2005-05-10 | 2006-11-16 | Xerox Corporation | Photoreceptors |
| CN104743543A (en) * | 2015-03-04 | 2015-07-01 | 同济大学 | Method for preparing polyaniline/phenolic aldehyde based carbon material |
| CN105895380A (en) * | 2016-04-12 | 2016-08-24 | 齐鲁工业大学 | Three-dimensional reticular polyaniline/phenolic resin-based carbon sphere composite material and preparation method thereof |
| CN107032320A (en) * | 2017-04-29 | 2017-08-11 | 成都博美实润科技有限公司 | A kind of preparation method based on polyaniline-modified phenolic resin base porous carbon |
| CN109289763A (en) * | 2018-10-24 | 2019-02-01 | 南京海洛阿姆生物科技有限公司 | A kind of cleanser and production technology removing formaldehyde in indoor air |
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