CN106423114A - Purification adsorbent for hydrocarbon impurities, preparing method and application - Google Patents
Purification adsorbent for hydrocarbon impurities, preparing method and application Download PDFInfo
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- 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
- B01J20/18—Synthetic zeolitic molecular sieves
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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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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
- B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3408—Regenerating or reactivating of aluminosilicate molecular sieves
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
- C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/24—Hydrocarbons
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a purification adsorbent for removing impurities in polymerized olefin materials prepared from coal through methyl alcohol. The purification adsorbent for hydrocarbon impurities is prepared from, by weight, 20%-59.5% of molecular sieves, 0.5%-1% of metallic oxide and 40%-64% of activated aluminum oxide, wherein the molecular sieves are composite molecular sieves, and are prepared in the mode that an SAPO molecular sieve or SSZ molecular sieve and one or more of a A-type molecular sieve, X-type molecular sieve and Y-type molecular sieve are mixed. Compared with the prior art, the adsorbent prepared with the method is high in particle mechanical strength, small in dust and low in adsorption heat effect, has the deep adsorption function, and can be used for removing impurities such as water, carbon dioxide, hydrogen sulfide, methyl alcohol, ethyl alcohol, formaldehyde, acetaldehyde, mercaptan and dimethyl ether in the polymerized olefin materials prepared from the coal through the methyl alcohol.
Description
Technical field：
The invention belongs to purifying adsorbent field, it is used for removing coal through impurity in methanol olefin polymerization material particularly to one kind
Purifying adsorbent.
Background technology：
Coal opens the Article 2 technique for producing raw material route of alkene production through methanol olefin polymerization.With traditional petroleum cracking
Technique is different, no matter wherein the ethylene of production, the impurity in propylene are in species or content, all differs larger.For coal warp
The ethylene of methanol production, propylene will reach the quality level of the aggregation level of petroleum cracking technique, the first in purification ethylene, propylene
The oxycompound impurity such as alcohol, ethanol, dimethyl ether is that coal purifies emphasis and the key of technique through methanol-to-olefins.And low-cost net
Changing alkene becomes the focus of concern universal at present.
Molecular sieve, aluminium oxide, as solid absorbent, are frequently used for miscellaneous in the logistics such as purification separation alkene, natural gas
Matter.It has been reported that using molecular sieve or aluminium oxide come the oxycompound impurity such as methanol, dimethyl ether in purification of light olefins, alkene is insatiable hunger
And hydrocarbon, there is stronger polarity, in above-mentioned alkene, impurity is also polar molecule, when purifying impurity using molecular sieve adsorption, simultaneously
Alkene can be adsorbed, cause adsorbent bed to heat up, and then cause alkene in adsorbent surface polymerism.When aluminium oxide does adsorbent,
Though heat of adsorption is low, there is adsorption deeply and all low defect of capacity.
Content of the invention
The purpose of the present invention is to overcome above-mentioned deficiency problem, provides one kind to be used for hydrocarbon impurities purifying adsorbent, has relatively
Low absorption heat effect, has the ability of high power capacity depth adsorbing contaminant simultaneously again, can deviate from multiple poles from olefin stream simultaneously
Property impurity, the such as oxycompound such as methanol, ethanol, dimethyl ether, still have the ability of preferable adsorbing contaminant after repeatedly regenerating.The present invention
Another object is that offer is a kind of and be used for hydrocarbon impurities purifying adsorbent, process is simple is it is ensured that properties of product.The 3rd of the present invention
Individual purpose is to provide a kind of application for hydrocarbon impurities purifying adsorbent, applies most suitable field, and effect reaches most preferably.
The present invention can be achieved through the following technical solutions：A kind of be used for hydrocarbon impurities purifying adsorbent, adsorbent by point
Son sieve, metal-oxide and activated alumina are made, and each parts by weight of raw materials ratio is：Molecular sieve 20-59.5%, rare earth oxide
0.5%-1%, aluminium oxide 40-64%, wherein molecular sieve are complex type molecular sieves, by SAPO molecular sieve or SSZ molecular sieve, then with A type
One or more of molecular sieve, X-type molecular sieve and Y type molecular sieve mix.
Described adsorbent preferred molecular sieve 35-59%, rare earth oxide 0.5%-1%, aluminium oxide 40-64%.
Described adsorbent is in the granule of spherical shape, and diameter is between 1-5mm.
The crystal structure of described aluminium oxide powder is γ-Al2O3, specific surface area is more than 200m2/g.
Between 1-4um, the content of wherein SAPO or SSZ molecular sieve accounts for absorption to the particle size of described raw molecule sieve
The 5-10% of agent gross weight.
Described rare earth oxide is lanthana（La2O3）Or cerium oxide (Ce2O3) etc..
A kind of preparation method for hydrocarbon impurities purifying adsorbent of the present invention it is characterised in that：Preparation process is as follows：
（1）Molecular sieve, alumina powder, rare earth oxide are sufficiently mixed by mechanical agitation；
（2）After mixing, material adds in pot forming, and rotational forming in pot forming rotation process, sprays into binding agent, makes graininess
Adsorbent, wherein binding agent water spray into the 15-20% that weight accounts for,
（3）Granular adsorbent is dried, and for room temperature to 200 degrees Celsius, drying time is 0.5 to 2 hours to baking temperature；
（4）Dried granular adsorbent is activated again, and activation temperature is 200 to 500 degrees Celsius, and soak time is 0.5
By 3 hours, prepared finished product adsorbent.
A kind of application for hydrocarbon impurities purifying adsorbent of the present invention, adsorbent be used for hydrocarbon raw material in removing alcohol, ether,
CO2、The purification of the impurity such as water, particularly preferred for the removing purification through impurity in methanol olefin polymerization material for the coal.
The present invention compared with similar products, has prominent substantive distinguishing features and significantly improves, be embodied in：
（1）Another composition of adsorbent of the present invention is molecular sieve, acts primarily as the effect of adsorbing contaminant.Molecular sieve is that one kind has
The water-containing crystal aluminosilicate of homogeneous micropore, application the present invention be SAPO molecular sieve or SSZ molecular sieve, then with A type molecular sieve,
One or more of X-type molecular sieve and Y type molecular sieve mix, and wherein SSZ, SAPO molecular sieve topological structure are CHA type.Molecule
Sieve is sufficiently mixed with aluminium oxide, enables liberated heat during molecular sieve adsorption impurity to disperse in time to be released, it is to avoid molecule
Sieve adsorbent bed temperature runaway causes olefinic polymerization phenomenon.
（2）The present invention adds micro rare earth oxide, and the stability of adsorbent has been significantly greatly increased.Hot conditionss are difficult to burn
Knot and phase transformation, anti-carbon deposition ability also dramatically increases.
（3）The necessary component of adsorbent of the present invention is activated alumina, and its crystal phase structure is γ-Al2O3, permissible
It is activated alumina powder on the market, specific surface area is more than 200m2/ g, raw material is easy to get, and effect is good.
Final finished adsorbent can remove multiple pollutant in olefin feed, and these olefin feed contain：Water, titanium dioxide
The oxygenatedchemicalss such as carbon, alcohol, ether, aldehyde, one kind of the sulfur-containing compound such as hydrogen sulfide, mercaptan and multiple pollutant.
Application effect of the present invention is notable, contacts to purify alkene with adsorbent using continuous way fixed bed olefin stream.Alkene
Material should carry out activation procedure to adsorbent before contacting with adsorbent, and the nitrogen being dried is passed through with certain temperature and air speed
Adsorbent bed heating adsorbent.Between 250-350 degree, air speed is less than 8000/H to temperature control, through adsorbent activation
Afterwards, raw material olefin material is contacted with adsorbent and is cleaned.
Brief description：
Fig. 1 is the XRD figure spectrogram of inventive samples 1#.
Specific embodiment：
With reference to example, the present invention is described in detail.
Embodiment 1
One kind is used for hydrocarbon impurities purifying adsorbent, and adsorbent is made up of molecular sieve, metal-oxide and activated alumina, each former
Material weight aluminium oxide 150g, 13X molecular sieve 110g and SAPO-34 molecular sieve 10g and rare earth oxide La2O31.5g；
Preparation process is as follows：
（1）Molecular sieve, alumina powder, rare earth oxide are sufficiently mixed by mechanical agitation for 20 minutes；
（2）After mixing, material adds in pot forming, and rotational forming, in pot forming rotation process, slowly sprays into binding agent deionization
Water 100g, makes granular adsorbent；
（3）Granular adsorbent is dried, and baking temperature is 100 degrees Celsius, and drying time is 2 hours；
（4）Dried granular adsorbent is activated again, and activation temperature is 450-480 degree Celsius, and soak time is little for 1
When, prepared finished product adsorbent（Sample 1#）.
Embodiment 2
One kind is used for hydrocarbon impurities purifying adsorbent, and adsorbent is made up of molecular sieve, metal-oxide and activated alumina, each former
Material weight：Aluminium oxide 160g, 5A molecular sieve 140g, SAPO-34 molecular sieve 20g, powder shape rare earth oxide Ce2O32g；
Concrete preparation technology, with embodiment 1, makes sample 2#.
Embodiment 3
One kind is used for hydrocarbon impurities purifying adsorbent, and adsorbent is made up of molecular sieve, metal-oxide and activated alumina, each former
Material weight：Aluminium oxide 200g and SSZ molecular sieve 25g, 13X molecular sieve 95g, NaY molecular sieve 60g, rare earth oxide La2O32.5
g；
Concrete preparation technology, with embodiment 1, makes sample 3#
Embodiment 4
One kind is used for hydrocarbon impurities purifying adsorbent, and adsorbent is made up of molecular sieve, metal-oxide and activated alumina, each former
Material weight：Aluminium oxide 120g and SSZ molecular sieve 8g, NaY molecular sieve 72g, rare earth oxide La2O31.5 g；
Each raw material above is sufficiently mixed, puts into water spray molding in disk rotational forming machine, 1-3mm spherical particle is chosen in screening,
Put into electric oven to be dried, 120 degree of baking temperature, time 2 h；Then muffle furnace activation, 460 degree of activation temperature, the time 1 is little
When；Make sample 4#.
Embodiment 5
One kind is used for hydrocarbon impurities purifying adsorbent, and adsorbent is made up of molecular sieve, metal-oxide and activated alumina, each former
Material weight：Aluminium oxide 130g and SSZ molecular sieve 8g, 13X molecular sieve 72g, rare earth oxide La2O31.5 g；
Each raw material above is sufficiently mixed, puts into water spray molding in disk rotational forming machine, 1-3mm spherical particle is chosen in screening,
Put into electric oven to be dried, 120 degree of baking temperature, time 2 h；Then muffle furnace activation, 480 degree of activation temperature, the time 1 is little
When；Make sample 5#.
Dynamic evaluation is carried out to above-mentioned prepared adsorbent, under actual condition state, the evaluation of adsorbent adsorbing contaminant capacity.
Take sample of sorbent 1# 10g, 2# 10g, 4#10g are respectively charged into gas phase evaluating apparatus.In about 500/h high pure nitrogen
Under flow, 300 DEG C activate 2 hours, then cool down room temperature.Using containing trace impurity（Methanol：200ppm, dimethyl ether：200ppm、）
High pure nitrogen, continues through adsorbent bed with 600ml/min flow velocity, the pressure of 0.1MPa, the tail gas through over-molecular sieve, using color
The content of spectrometer checked for impurities.Investigate the adsorbance to impurity for the adsorbent.
Sample of sorbent 3# 10g, 5# 10g is taken to be respectively charged into gas phase evaluating apparatus.In about 500/h high pure nitrogen flow
Under, 300 DEG C activate 2 hours, then cool down room temperature.Using containing trace impurity（Methanol：200ppm, dimethyl ether：200ppm、）High-purity
Nitrogen, continues through adsorbent bed with 1200ml/min flow velocity, the pressure of 0.1MPa, the tail gas through over-molecular sieve, using chromatograph
The content of instrument checked for impurities.Investigate the adsorbance to impurity for the adsorbent.
Above testing inspection result such as table 1
Table 1
| Sample number into spectrum | Flow velocity ml/min | Time of break-through min | Adsorb miscellaneous capacity mg/g |
| 1# | 600 | 660 | 40 |
| 2# | 600 | 600 | 35 |
| 3# | 1200 | 300 | 36 |
| 4# | 600 | 555 | 30 |
| 5# | 1200 | 335 | 38 |
Degradation, evaluates the change of adsorbent reactivation number of times and adsorption capacity
By the evaluation methodology of sample 1#, sample 1#, sample 3#, the continuous absorption regeneration of sample 4# 100 times, investigate the absorption of adsorbent
Amount down ratio.
Above testing inspection result such as table 2
Table 2
| Sample number into spectrum | Regeneration times | Adsorbing contaminant capacity mg/g | Adsorbance rate of descent % |
| 1# | 100 | 36.5 | 8.7 |
| 3# | 100 | 32.4 | 10 |
| 4# | 100 | 27.15 | 9.5 |
Claims (8)
1. a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Adsorbent is by molecular sieve, metal-oxide and active oxygen
Change aluminum to make, each parts by weight of raw materials ratio is：Molecular sieve 20-59.5%, rare earth oxide 0.5%-1%, aluminium oxide 40-64%, wherein
Molecular sieve is complex type molecular sieve, by SAPO molecular sieve or SSZ molecular sieve, then with A type molecular sieve, X-type molecular sieve and Y type molecule
The mixing of one or more of sieve.
2. according to claim 1 a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Described adsorbent is preferred
Molecular sieve 35-59%, rare earth oxide 0.5%-1%, aluminium oxide 40-64%.
3. according to claim 1 and 2 a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Described absorption
Agent is in the granule of spherical shape, and diameter is between 1-5mm.
4. according to claim 1 and 2 a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Described oxidation
The crystal structure of aluminium powder foam is γ-Al2O3, specific surface area is more than 200m2/g.
5. according to claim 1 and 2 a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Described raw material
The particle size of molecular sieve between 1-4um, wherein SAPO, content relative adsorption agent weight 5-10% of SSZ molecular sieve.
6. according to claim 1 and 2 a kind of for hydrocarbon impurities purifying adsorbent it is characterised in that：Described rare earth oxygen
Compound is lanthana or cerium oxide etc..
7. a kind of preparation method for hydrocarbon impurities purifying adsorbent it is characterised in that：Preparation process is as follows：
（1）Molecular sieve, alumina powder, rare earth oxide are sufficiently mixed by mechanical agitation；
（2）After mixing, material adds in pot forming, and rotational forming in pot forming rotation process, sprays into binding agent, makes graininess
Adsorbent, wherein binding agent water spray into the 15-20% that weight accounts for,
（3）Granular adsorbent is dried, and for room temperature to 200 degrees Celsius, drying time is 0.5 to 2 hours to baking temperature；
（4）Dried granular adsorbent is activated again, and activation temperature is 200 to 500 degrees Celsius, and soak time is 0.5
By 3 hours, prepared finished product adsorbent.
8. a kind of application for hydrocarbon impurities purifying adsorbent it is characterised in that：Adsorbent be used for hydrocarbon raw material in removing alcohol,
Ether, CO2、The purification of the impurity such as water, is preferred for removing the purification through impurity in methanol olefin polymerization material for the coal.
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| CN108033460A (en) * | 2017-12-26 | 2018-05-15 | 大连海鑫化工有限公司 | A kind of new 3A molecular sieves and preparation method thereof |
| CN108246249A (en) * | 2018-02-13 | 2018-07-06 | 大连海鑫化工有限公司 | It is a kind of to be used to remove adsorbent of the low thermal discharge of polar molecule in material and preparation method thereof |
| CN108499526A (en) * | 2018-01-16 | 2018-09-07 | 奥斯催化材料（大连)有限公司 | A kind of preparation and application for removing the adsorbent of impurity in propylene oxide stream |
| CN109759009A (en) * | 2019-03-07 | 2019-05-17 | 朱江凤 | Dimethyl ether adsorbent and the preparation method and application thereof |
| CN111468181A (en) * | 2020-05-21 | 2020-07-31 | 南京诚志清洁能源有限公司 | Composite catalyst for improving reaction stability of methanol-to-olefin and application thereof |
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| CN114433011A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Adsorbent for removing nitride in aromatic hydrocarbon and preparation method and application thereof |
| CN114939324A (en) * | 2022-05-26 | 2022-08-26 | 广西电网有限责任公司电力科学研究院 | Suspension type power switch cabinet gas adsorption device |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108033460A (en) * | 2017-12-26 | 2018-05-15 | 大连海鑫化工有限公司 | A kind of new 3A molecular sieves and preparation method thereof |
| CN108499526A (en) * | 2018-01-16 | 2018-09-07 | 奥斯催化材料（大连)有限公司 | A kind of preparation and application for removing the adsorbent of impurity in propylene oxide stream |
| CN108499526B (en) * | 2018-01-16 | 2021-04-27 | 奥斯催化材料（大连)有限公司 | Preparation and application of adsorbent for removing impurities in propane material flow |
| CN108246249A (en) * | 2018-02-13 | 2018-07-06 | 大连海鑫化工有限公司 | It is a kind of to be used to remove adsorbent of the low thermal discharge of polar molecule in material and preparation method thereof |
| CN109759009A (en) * | 2019-03-07 | 2019-05-17 | 朱江凤 | Dimethyl ether adsorbent and the preparation method and application thereof |
| CN111468181A (en) * | 2020-05-21 | 2020-07-31 | 南京诚志清洁能源有限公司 | Composite catalyst for improving reaction stability of methanol-to-olefin and application thereof |
| WO2022063259A1 (en) * | 2020-09-28 | 2022-03-31 | 中国石油化工股份有限公司 | Adsorbent composition, and preparation method therefor and application thereof |
| CN114425296A (en) * | 2020-09-28 | 2022-05-03 | 中国石油化工股份有限公司 | Adsorbent for removing polar compounds in olefin and preparation method and application thereof |
| CN114433011A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Adsorbent for removing nitride in aromatic hydrocarbon and preparation method and application thereof |
| CN114433011B (en) * | 2020-10-20 | 2023-07-04 | 中国石油化工股份有限公司 | Adsorbent for removing nitride in aromatic hydrocarbon and preparation method and application thereof |
| CN114939324A (en) * | 2022-05-26 | 2022-08-26 | 广西电网有限责任公司电力科学研究院 | Suspension type power switch cabinet gas adsorption device |
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| CN106423114B (en) | 2019-09-20 |
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