CN107670644A - A kind of preparation method of pyridine adsorption agent - Google Patents
A kind of preparation method of pyridine adsorption agent Download PDFInfo
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- CN107670644A CN107670644A CN201711069394.6A CN201711069394A CN107670644A CN 107670644 A CN107670644 A CN 107670644A CN 201711069394 A CN201711069394 A CN 201711069394A CN 107670644 A CN107670644 A CN 107670644A
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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
Abstract
The invention discloses a kind of preparation method of pyridine adsorption agent, comprise the following steps：1）The NaY molecular sieve original sphere of powder is ground first and mixed with alumina silicate, is placed in heat-activated in Muffle furnace；2）By the mixed powder after activation, roasting, broken obtained cylindrical pellet after extruded moulding；3）Cylindrical pellet is immersed in zeolite powder suspension；4）Then fumigated 12 hours in 110 200 DEG C of water vapour；Then dry 23 hours at 100 120 DEG C, be calcined 58 hours at 550 580 DEG C, pyridine adsorption agent is made；Pyridine adsorption agent prepared by the present invention is to pyridine with good adsorption effect, with advanced nitrogen ability.
Description
Technical field
The present invention relates to a kind of preparation method of pyridine adsorption agent.
Background technology
Pyridine, organic compound, it is the 6-membered heterocyclic compound containing a nitrogen heteroatom.It can regard as in benzene molecular
One（CH）The compound substituted by N, therefore also known as pyridine, colourless or slightly yellow liquid, foul smelling.Pyridine and its homologue are present
In Dippel's oil, coal tar, coal gas, shale oil, oil.Pyridine industrially can be used as denaturant, dyeing auxiliaries, and synthesis one
Series of products（Including medicine, disinfectant, dyestuff etc.）Raw material.
Typical Representative of the pyridine as heterocyclic organic compound, is deposited extensively in the industrial wastewaters such as agricultural chemicals, medicine, chemical industry
Triggering serious problem of environmental pollution.Further, since the high toxicity and difficult for biological degradation characteristic of pyridine, pyridine pollution
Improvement has very big technical difficulty.Absorption method, because its operating cost is low, adsorption capacity is strong, and regenerating easily, has become
One of effective ways of organic wastewater are handled, therefore there is an urgent need to develop a kind of pyridine with stronger advanced nitrogen ability
Adsorbent.
The content of the invention
The technical problems to be solved by the invention are the shortcomings that overcoming above prior art：There is provided a kind of has to pyridine
Good adsorption effect, have advanced nitrogen ability pyridine adsorption agent preparation method.
The technical solution of the present invention is as follows：A kind of preparation method of pyridine adsorption agent, comprises the following steps：
1）It is 2-6 microns that the NaY molecular sieve original sphere of powder is milled into average grain diameter first, with the alumina silicate that granularity is 0.5-0.8 microns
By weight 100:（2-8）Ratio mixing, be placed in heat-activated in Muffle furnace；
2）By step 1）Mixed powder after activation, less than 40 DEG C are cooled to, add binding agent and deionized water mixing, mediate, squeeze
Bar shaping is calcined 4-6 hours at 450-480 DEG C, broken is made cylindric after drying 1-2 hours at 100-120 DEG C
Grain；
3）By step 2）Prepared cylindrical pellet, it is immersed in and filters out liquid after 1-3 minutes in zeolite powder suspension and obtain
The particle of zeolite slurry is soaked with into duct, wherein zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is 100-
200nm clinoptilolite powder 13-24 parts, granularity be 50-80nm chabasie powder 7-10 parts, deionized water 100-150 parts；
4）By step 3）The particle that zeolite slurry is soaked with middle duct fumigates 1-2 hours in 110-200 DEG C of water vapour；Then
2-3 hours are dried at 100-120 DEG C, 5-8 hours are calcined at 550-580 DEG C, pyridine adsorption agent is made.
As optimization, step 1）In, activation temperature is 430-460 DEG C, soak time 4-6 hours.
As optimization, step 3）In, zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is 100-200nm
15 parts of clinoptilolite powder, granularity be 50-80nm 8 parts of chabasie powder, 100 parts of deionized water.
As optimization, the binding agent is sodium carboxymethylcellulose.
The beneficial effects of the invention are as follows：The present invention by zeolite materials by immersing the molecular sieve activated by alumina silicate
Grain duct, sinters the good crystalline phase tissue of realization after then being fumigated in water vapour, be effectively increased to the adsorption capacity of pyridine and
Adsorption capacity, by the absorption property and regenerability of pyridine adsorption agent after contrasting molecular screen primary powder and being molded, it is found that pyridine is inhaled
Attached dose penetrates treating capacity and decreases, but more stable to pyridine adsorption performance, and under identical adsorption conditionses, pyridine is inhaled
Attached dose has stronger advanced nitrogen ability than molecular screen primary powder.
Embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment one
A kind of preparation method of pyridine adsorption agent, comprises the following steps：
1）It is 2-6 microns that the NaY molecular sieve original sphere of powder is milled into average grain diameter first, with the alumina silicate that granularity is 0.5-0.8 microns
By weight 100:2 ratio mixing, is placed in heat-activated in Muffle furnace；Activation temperature is 430-460 DEG C, soak time 4-6
Hour.
2）By step 1）Mixed powder after activation, is cooled to room temperature, add sodium carboxymethylcellulose and deionized water mixing,
Kneading, extruded moulding are calcined 6 hours, broken obtained cylindrical pellet after being dried 2 hours at 120 DEG C at 480 DEG C；Institute
The weight ratio for stating sodium carboxymethylcellulose and mixed powder is 1:6-8.
3）By step 2）Prepared cylindrical pellet, it is immersed in zeolite powder suspension and filters out liquid after 3 minutes
Obtain being soaked with the particle of zeolite slurry in duct, wherein zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is
13 parts of 100-200nm clinoptilolite powder, granularity be 50-80nm 10 parts of chabasie powder, 100 parts of deionized water；
4）By step 3）The particle that zeolite slurry is soaked with middle duct is fumigated 1 hour in 200 DEG C of water vapour；Then in 100
Dry 3 hours at DEG C, be calcined 8 hours at 580 DEG C, pyridine adsorption agent is made.
Embodiment two
A kind of preparation method of pyridine adsorption agent, comprises the following steps：
1）It is 2-6 microns that the NaY molecular sieve original sphere of powder is milled into average grain diameter first, with the alumina silicate that granularity is 0.5-0.8 microns
By weight 100:8 ratio mixing, is placed in heat-activated in Muffle furnace；Activation temperature is 460 DEG C, soak time 6 hours.
2）By step 1）Mixed powder after activation, less than 40 DEG C are cooled to, add binding agent and deionized water mixing, pinch
Conjunction, extruded moulding are calcined 4-6 hours, broken obtained cylinder after drying 1-2 hours at 100-120 DEG C at 450-480 DEG C
Shape particle；The weight ratio of the binding agent and mixed powder is 1:6.
3）By step 2）Prepared cylindrical pellet, it is immersed in zeolite powder suspension and filters out liquid after 3 minutes
Obtain being soaked with the particle of zeolite slurry in duct, wherein zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is
15 parts of 100-200nm clinoptilolite powder, granularity be 50-80nm 8 parts of chabasie powder, 100 parts of deionized water.
4）By step 3）The particle that zeolite slurry is soaked with middle duct is fumigated 2 hours in 110 DEG C of water vapour；Then in
Dry 3 hours at 120 DEG C, be calcined 8 hours at 580 DEG C, pyridine adsorption agent is made.
Embodiment three
A kind of preparation method of pyridine adsorption agent, comprises the following steps：
1）It is 2-6 microns that the NaY molecular sieve original sphere of powder is milled into average grain diameter first, with the alumina silicate that granularity is 0.5-0.8 microns
By weight 100:5 ratio mixing, is placed in heat-activated in Muffle furnace；Activation temperature is 450 DEG C, soak time 5 hours.
2）By step 1）Mixed powder after activation, room temperature is cooled to, it is 1 to add with the mixed powder weight ratio after activation:5
The mixing of the deionized water of sodium carboxymethylcellulose and powder gross weight 25%, kneading, extruded moulding are small after drying 2 at 120 DEG C
When, 5 hours, broken obtained cylindrical pellet are calcined at 450 DEG C；
3）By step 2）Prepared cylindrical pellet, it is immersed in and filters out liquid after 1 minute in zeolite powder suspension and obtain
The particle of zeolite slurry is soaked with duct, wherein zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is 100-
15 parts of 200nm clinoptilolite powder, granularity be 50-80nm 8 parts of chabasie powder, 100 parts of deionized water.
4）By step 3）The particle that zeolite slurry is soaked with middle duct fumigates 1-2 hours in 110-200 DEG C of water vapour；
Then dry 3 hours at 100 DEG C, be calcined 8 hours at 580 DEG C, pyridine adsorption agent is made.
It the above is only the feature implementation example of the present invention, the scope of the present invention be not limited in any way.It is all to use together
The technical scheme formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (4)
- A kind of 1. preparation method of pyridine adsorption agent, it is characterised in that：Comprise the following steps：1）It is 2-6 microns that the NaY molecular sieve original sphere of powder is milled into average grain diameter first, with the alumina silicate that granularity is 0.5-0.8 microns By weight 100:（2-8）Ratio mixing, be placed in heat-activated in Muffle furnace；2）By step 1）Mixed powder after activation, less than 40 DEG C are cooled to, add binding agent and deionized water mixing, mediate, squeeze Bar shaping is calcined 4-6 hours at 450-480 DEG C, broken is made cylindric after drying 1-2 hours at 100-120 DEG C Grain；3）By step 2）Prepared cylindrical pellet, it is immersed in and filters out liquid after 1-3 minutes in zeolite powder suspension and obtain The particle of zeolite slurry is soaked with into duct, wherein zeolite powder suspension is made up of the raw material of following parts by weight：Granularity is 100- 200nm clinoptilolite powder 13-24 parts, granularity be 50-80nm chabasie powder 7-10 parts, deionized water 100-150 parts；4）By step 3）The particle that zeolite slurry is soaked with middle duct fumigates 1-2 hours in 110-200 DEG C of water vapour；Then 2-3 hours are dried at 100-120 DEG C, 5-8 hours are calcined at 550-580 DEG C, pyridine adsorption agent is made.
- 2. the preparation method of pyridine adsorption agent according to claim 1, it is characterised in that：Step 1）In, activation temperature For 430-460 DEG C, soak time 4-6 hours.
- 3. the preparation method of pyridine adsorption agent according to claim 1, it is characterised in that：Step 3）In, zeolite powder hangs Supernatant liquid is made up of the raw material of following parts by weight：Granularity is 100-200nm 15 parts of clinoptilolite powder, and granularity is 50-80nm water chestnut 8 parts of zeolite powder, 100 parts of deionized water.
- 4. the preparation method of pyridine adsorption agent according to claim 1, it is characterised in that：The binding agent is that carboxymethyl is fine Tie up plain sodium.
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| CN201711069394.6A CN107670644A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of pyridine adsorption agent |
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| CN201711069394.6A CN107670644A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of pyridine adsorption agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045419A (en) * | 2021-03-24 | 2021-06-29 | 西南化工研究设计院有限公司 | Preparation method and application of catalyst for removing pyridine from crude methyl acetate |
Citations (5)
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|---|---|---|---|---|
| CN1303735A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Molecular sieve carbon fabric for separating methane from carbon dioxide and its preparation method |
| CN1806908A (en) * | 2005-10-27 | 2006-07-26 | 复旦大学 | Macroporous zeolite absorbent and preparation method thereof |
| CN101007261A (en) * | 2006-12-17 | 2007-08-01 | 于向真 | Zeolite adsorbent and its preparation method |
| CN103037963A (en) * | 2010-06-10 | 2013-04-10 | 多种吸附技术公司 | Chabazite and clinoptilolite in oxygen absorbers |
| CN106861610A (en) * | 2017-04-12 | 2017-06-20 | 明光市国星凹土有限公司 | A kind of preparation method containing bentone adsorbent |
-
2017
- 2017-11-03 CN CN201711069394.6A patent/CN107670644A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303735A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Molecular sieve carbon fabric for separating methane from carbon dioxide and its preparation method |
| CN1806908A (en) * | 2005-10-27 | 2006-07-26 | 复旦大学 | Macroporous zeolite absorbent and preparation method thereof |
| CN101007261A (en) * | 2006-12-17 | 2007-08-01 | 于向真 | Zeolite adsorbent and its preparation method |
| CN103037963A (en) * | 2010-06-10 | 2013-04-10 | 多种吸附技术公司 | Chabazite and clinoptilolite in oxygen absorbers |
| CN106861610A (en) * | 2017-04-12 | 2017-06-20 | 明光市国星凹土有限公司 | A kind of preparation method containing bentone adsorbent |
Non-Patent Citations (1)
| Title |
|---|
| 牛丛丛等: ""吸附法分离焦化甲苯中的吡啶类物质及吸附剂的再生"", 《化工进展》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045419A (en) * | 2021-03-24 | 2021-06-29 | 西南化工研究设计院有限公司 | Preparation method and application of catalyst for removing pyridine from crude methyl acetate |
| CN113045419B (en) * | 2021-03-24 | 2022-03-08 | 西南化工研究设计院有限公司 | Preparation method and application of catalyst for removing pyridine from crude methyl acetate |
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