CN108079943A - A kind of preparation method with superelevation mesoporous spheric active carbon - Google Patents

A kind of preparation method with superelevation mesoporous spheric active carbon Download PDF

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CN108079943A
CN108079943A CN201611031994.9A CN201611031994A CN108079943A CN 108079943 A CN108079943 A CN 108079943A CN 201611031994 A CN201611031994 A CN 201611031994A CN 108079943 A CN108079943 A CN 108079943A
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exchange resin
ion exchange
resin ball
active carbon
mesoporous
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曹建涛
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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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28078—Pore diameter

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to a kind of preparation methods with superelevation mesoporous spheric active carbon, belong to activated carbon field, and its preparation method is：Ion exchange resin ball is prepared using techniques such as deionized water swelling, catalyst crosslinking, ageing and high temperature cabonizations.The spheric active carbon prepared using the method for the present invention is simple for process, environmental-friendly, has superelevation mesoporous and high specific surface area, suitable for large-scale production.

Description

A kind of preparation method with superelevation mesoporous spheric active carbon
Technical field
The invention belongs to a kind of preparation methods of activated carbon, relate in particular to a kind of system of high mesoporosity spheric active carbon Preparation Method.
Background technology
Spheric active carbon due to high-specific surface area, excellent sphericity, higher mechanical strength and acid and alkali-resistance and A series of good characteristics such as high temperature resistant can be widely applied to the fields such as medical treatment, environmental protection, chemical defence, gas separation and solvent recovery. Field of blood purification, spheric active carbon also need absorption middle molecule toxins in addition to adsorbing small molecule toxins, and this requires spherical Activated carbon has higher mesoporous.Lv Chunxiang (patent publication No.s：) etc. CN1480397A spherical resin is used as raw material, pass through Swelling, depth sulfonation, gradient concentration pickling, charing and activation are prepared for spheric active carbon.Although using depth process for sulfonation energy The pore structure of spherical resin is enough kept, prepares the spheric active carbon of high mesoporosity, but depth process for sulfonation needs are substantial amounts of dense The presence of sulfuric acid, acid pickle and sour gas be easy to cause environmental pollution, while larger corrosion is caused to equipment, is unfavorable for work Industry metaplasia is produced.Ling Licheng (patent publication No.s：) etc. CN1480399A spherical resin is used as raw material, at air pre-oxidation Reason carbonizes and activation is prepared for spheric active carbon again.Although air pre-oxidation process can prepare the spherical work rich in mesoporous Property charcoal, but air pre-oxidation process power consumption is big, process cycle is long, and the oxidation uniformity coefficient of spherical resin is difficult to control, unfavorable In large-scale production.Qi Hongyun (patent publication No.s：) etc. CN1631516 macroporous type bead is copolymerized using styrene-divinylbenzene For raw material, spheric active carbon is prepared for by series of process routes such as chloromethylation, Friedel-crafts reaction, stabilisation and activation.Though High intensity, the spheric active carbon of high mesoporosity so can be prepared in this way, and can be mass produced, but chloromethane Base and Friedel-crafts reaction need two kinds of hypertoxicity solvents of chloromethylether and nitrobenzene, and human body and environment are caused to be difficult to the injury recovered Or pollution.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of process route is simple, processing step is few, environmental-friendly, has The preparation method of superelevation mesoporous spheric active carbon.
The present invention uses the ion exchange resin ball of commercialization as raw material, can be sent out in water using ion exchange resin ball The mechanism of raw swelling promotes the deep-crosslinked of molecular resin using catalyst, so as to control the pore structure of gained Carbon Materials, and then Direct high temperature cabonization prepares the spheric active carbon of superelevation mesoporous.It concretely comprises the following steps：
1. the expansion of ion exchange resin ball：100g ion exchange resin dry bulbs are placed in and fill 200-500ml deionizations In the beaker of water, when water temperature is 50-70 DEG C, magnetic agitation 0.5-2h is swollen.
2. the catalytic crosslinking of ion exchange resin ball：The catalysis of 10-30g is added dropwise in above-mentioned ion exchange resin ball solution Agent, and react 1-3h when water temperature is 50-70 DEG C.
3. the ageing of ion exchange resin ball：The beaker for filling above-mentioned ion exchange resin ball is placed in 20-30 DEG C of temperature Under carry out ageing 5-10h.
4. the drying of ion exchange resin ball：The solution of above-mentioned ion exchange resin ball will be filled at a temperature of 15-25 DEG C Separation of solid and liquid is carried out using Buchner funnel.Then ion exchange resin ball is placed in 100-105 DEG C of baking oven dry 2-5h.
5. the high temperature carbonization of ion exchange resin ball：The ion exchange resin ball of above-mentioned drying is placed in tube furnace and is being flowed Speed is carbonized to be warming up to 900-1100 DEG C under the nitrogen protection of 50-100ml/min with the rate of 1-3 DEG C/min, and herein At a temperature of constant temperature 1-5h, then natural cooling is up to high mesoporosity spheric active carbon.
Ion exchange resin ball as described above is macroporous type styrene type cation exchange resin ball.
Catalyst as described above is Toluene-2,4-diisocyanate, any one in 4- diisocyanate, methyl diphenylene diisocyanate Kind.
Ion exchange resin as described above：Water：The mass ratio of toluene-catalyst is：10:20-50:1-3.
The technological progress obtained using the above-mentioned technical proposal present invention is：
This process route compares other process routes, and there is no the solvents for using the severe corrosives such as acid, alkali, reduce useless The discharge of liquid and the corrosion to equipment, have the advantages that environmental-friendly.Meanwhile this technique decreases air oxidation, vapor The time consuming process such as activation have the advantages that simple for process, processing step is few, suitable industrialized production.
Spheric active carbon prepared by this method has high mesoporosity (85%-93%) and high specific surface area (650- 1150m2/g)。
Specific embodiment
Embodiment 1：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing sulfonate radical is placed in and fills 200ml deionized waters In beaker, when water temperature is 50 DEG C, magnetic agitation 2h is expanded.Then 10g is added dropwise in above-mentioned ion exchange resin ball solution Toluene-2,4-diisocyanate, 4- diisocyanate, and react 3h when water temperature is 50 DEG C.And then the beaker that above-mentioned ion exchange resin ball will be filled 5h is aged at a temperature of being placed in 30 DEG C.Then the solution for filling above-mentioned ion exchange resin ball is leaked using Bu Shi at a temperature of 15 DEG C Bucket carries out separation of solid and liquid, and ion exchange resin ball is placed in 100 DEG C of baking ovens dry 2h.Finally by dry amberlite Fat ball is placed in tube furnace and is warming up to 900 DEG C of progress carbon under the nitrogen protection that flow velocity is 50ml/min with the rate of 1 DEG C/min Change, and constant temperature 5h at this temperature, then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous：85%；Specific surface Product：1150m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Embodiment 2：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing sulfonate radical is placed in and fills 300ml deionized waters In beaker, when water temperature is 55 DEG C, magnetic agitation 1.5h is expanded.Then it is added dropwise in above-mentioned ion exchange resin ball solution 15g Toluene-2,4-diisocyanates, 4- diisocyanate, and react 2.5h when water temperature is 55 DEG C.And then above-mentioned ion exchange resin ball will be filled Beaker be placed in 30 DEG C at a temperature of be aged 10h.Then the solution for filling above-mentioned ion exchange resin ball is adopted at a temperature of 20 DEG C Separation of solid and liquid is carried out with Buchner funnel, and ion exchange resin ball is placed in 105 DEG C of baking ovens dry 3h.Finally by it is dry from Sub-exchange resin ball is placed in tube furnace and is warming up under the nitrogen protection that flow velocity is 60ml/min with the rate of 1.5 DEG C/min 950 DEG C are carbonized, and constant temperature 4h at this temperature, and then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous： 87%；Specific surface area：1000m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Embodiment 3：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing carboxylate radical is placed in and fills 400ml deionized waters In beaker, when water temperature is 60 DEG C, magnetic agitation 1h is expanded.Then 20g is added dropwise in above-mentioned ion exchange resin ball solution Methyl diphenylene diisocyanate, and react 2h when water temperature is 60 DEG C.And then the burning that above-mentioned ion exchange resin ball will be filled Cup is aged 6h at a temperature of being placed in 25 DEG C.The solution for filling above-mentioned ion exchange resin ball is then used into Bu Shi at a temperature of 25 DEG C Funnel carries out separation of solid and liquid, and ion exchange resin ball is placed in 103 DEG C of baking ovens dry 2h.Finally by dry ion exchange Resin balls are placed in tube furnace and are warming up to 1000 DEG C of progress under the nitrogen protection that flow velocity is 70ml/min with the rate of 2 DEG C/min Carbonization, and constant temperature 3h at this temperature, then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous：88%；Compare table Area：910m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Embodiment 4：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing carboxylate radical is placed in and fills 500ml deionized waters In beaker, when water temperature is 65 DEG C, magnetic agitation 0.5h is expanded.Then it is added dropwise in above-mentioned ion exchange resin ball solution 25g Toluene-2,4-diisocyanates, 4- diisocyanate, and react 1.5h when water temperature is 65 DEG C.And then above-mentioned ion exchange resin ball will be filled Beaker be placed in 25 DEG C at a temperature of be aged 7h.Then the solution for filling above-mentioned ion exchange resin ball is used at a temperature of 15 DEG C Buchner funnel carries out separation of solid and liquid, and ion exchange resin ball is placed in 100 DEG C of baking ovens dry 2h.Finally by dry ion Exchange resin ball is placed in tube furnace and is warming up to 1050 under the nitrogen protection that flow velocity is 80ml/min with the rate of 2.5 DEG C/min It DEG C is carbonized, and constant temperature 2h at this temperature, then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous： 91%；Specific surface area：780m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Embodiment 5：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing sulfonate radical is placed in and fills 200ml deionized waters In beaker, when water temperature is 70 DEG C, magnetic agitation 2h is expanded.Then 30g is added dropwise in above-mentioned ion exchange resin ball solution Methyl diphenylene diisocyanate, and react 1h when water temperature is 70 DEG C.And then the burning that above-mentioned ion exchange resin ball will be filled Cup is aged 8h at a temperature of being placed in 20 DEG C.The solution for filling above-mentioned ion exchange resin ball is then used into Bu Shi at a temperature of 20 DEG C Funnel carries out separation of solid and liquid, and ion exchange resin ball is placed in 105 DEG C of baking ovens dry 2h.Finally by dry ion exchange Resin balls are placed in tube furnace and are warming up to 1100 DEG C of progress under the nitrogen protection that flow velocity is 90ml/min with the rate of 3 DEG C/min Carbonization, and constant temperature 1h at this temperature, then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous：93%；Compare table Area：650m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Embodiment 6：
The 100g macroporous type polystyrenes dry bulb of cation exchange resin containing carboxylate radical is placed in and fills 500ml deionized waters In beaker, when water temperature is 50 DEG C, magnetic agitation 0.5h is expanded.Then it is added dropwise in above-mentioned ion exchange resin ball solution 10g Toluene-2,4-diisocyanates, 4- diisocyanate, and react 1h when water temperature is 50 DEG C.And then above-mentioned ion exchange resin ball will be filled Beaker is aged 9h at a temperature of being placed in 20 DEG C.The solution for filling above-mentioned ion exchange resin ball is then used into cloth at a temperature of 25 DEG C Family name's funnel carries out separation of solid and liquid, and ion exchange resin ball is placed in 103 DEG C of baking ovens dry 5h.Finally dry ion is handed over It changes resin balls and is placed in tube furnace and with the rate of 1 DEG C/min be warming up to 1050 DEG C under the nitrogen protection that flow velocity is 100ml/min It is carbonized, and constant temperature 3h at this temperature, then natural cooling is up to superelevation mesoporous spheric active carbon (mesoporous：89%； Specific surface area：830m2/g).Spheric active carbon comparative example obtained by being not added with catalyst is shown in Table 1.
Table 1

Claims (6)

1. a kind of preparation method with superelevation mesoporous spheric active carbon, it is characterised in that include the following steps：
(1) expansion of ion exchange resin ball：100g ion exchange resin dry bulbs are placed in and fill 200-500ml deionized waters In beaker, when water temperature is 50-70 DEG C, magnetic agitation 0.5-2h is swollen；
(2) catalytic crosslinking of ion exchange resin ball：The catalyst of 10-30g is added dropwise in above-mentioned ion exchange resin ball solution, And react 1-3h when water temperature is 50-70 DEG C；
(3) ageing of ion exchange resin ball：At a temperature of the beaker for filling above-mentioned ion exchange resin ball is placed in 20-30 DEG C into Row ageing 5-10h；
(4) drying of ion exchange resin ball：The solution for filling above-mentioned ion exchange resin ball is used at a temperature of 15-25 DEG C Buchner funnel carries out separation of solid and liquid, and ion exchange resin ball is then placed in 100-105 DEG C of baking oven dry 2-5h；
(5) high temperature carbonization of ion exchange resin ball：The ion exchange resin ball of above-mentioned drying is placed in tube furnace in flow velocity It is carbonized to be warming up to 900-1100 DEG C under the nitrogen protection of 50-100ml/min with the rate of 1-3 DEG C/min, and it is warm herein The lower constant temperature 1-5h of degree, then natural cooling is up to high mesoporosity spheric active carbon.
A kind of 2. preparation method with superelevation mesoporous spheric active carbon according to claim 1, it is characterised in that institute The ion exchange resin ball stated is macroporous type styrene type cation exchange resin ball.
A kind of 3. preparation method with superelevation mesoporous spheric active carbon according to claim 2, it is characterised in that institute The macroporous type styrene type cation exchange resin ball stated is containing any type therein such as sulfonic group, carboxylic acid group.
A kind of 4. preparation method with superelevation mesoporous spheric active carbon according to claim 1, it is characterised in that institute The swelling temperature for the ion exchange resin ball stated is 50-70 DEG C.
A kind of 5. preparation method with superelevation mesoporous spheric active carbon according to claim 1, it is characterised in that institute The catalyst stated is Toluene-2,4-diisocyanate, any one in 4- diisocyanate, methyl diphenylene diisocyanate.
A kind of 6. preparation method with superelevation mesoporous spheric active carbon according to claim 1, it is characterised in that institute The ion exchange resin stated：Water：The mass ratio of catalyst is：10:20-50:1-3.
CN201611031994.9A 2016-11-19 2016-11-19 A kind of preparation method with superelevation mesoporous spheric active carbon Withdrawn CN108079943A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1480397A (en) * 2003-07-18 2004-03-10 中国科学院山西煤炭化学研究所 Method for preparing spherical active cardon with base of highstrength resin
CN102874806A (en) * 2012-09-26 2013-01-16 中国科学院山西煤炭化学研究所 Preparation method for spherical activated carbon with high bulk density and high specific surface area
CN105110330A (en) * 2015-08-17 2015-12-02 中国科学院上海高等研究院 Preparation method for activated carbon material and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1480397A (en) * 2003-07-18 2004-03-10 中国科学院山西煤炭化学研究所 Method for preparing spherical active cardon with base of highstrength resin
CN102874806A (en) * 2012-09-26 2013-01-16 中国科学院山西煤炭化学研究所 Preparation method for spherical activated carbon with high bulk density and high specific surface area
CN105110330A (en) * 2015-08-17 2015-12-02 中国科学院上海高等研究院 Preparation method for activated carbon material and application thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
WANG QIN ET.AL.: ""Preparation of polystyrene-based activated carbon spheres and their adsorption of dibenzothiophene"", 《NEW CARBON MATERIALS》 *
李存梅 等，: ""制备工艺对球状活性炭的影响研究"", 《化 工 新 型 材 料》 *
马跃敏 等，: ""甲苯二异氰酸酯改性乙烯基聚酯树脂"", 《华东化工学院学报》 *

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