CN104843699B - Method for preparing formed granular activated carbon for sugar solution decolorization by using waste powdered activated carbon - Google Patents
Method for preparing formed granular activated carbon for sugar solution decolorization by using waste powdered activated carbon Download PDFInfo
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- CN104843699B CN104843699B CN201510304122.4A CN201510304122A CN104843699B CN 104843699 B CN104843699 B CN 104843699B CN 201510304122 A CN201510304122 A CN 201510304122A CN 104843699 B CN104843699 B CN 104843699B
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Abstract
The invention discloses a method for preparing formed granular activated carbon for sugar solution decolorization by using waste powdered activated carbon, which comprises the following steps: completely dissolving one or more of soluble starch, polyvinyl alcohol, polyvinyl butyral and polyethyleneglycol in water as an additive, uniformly mixing the additive with coal tar, uniformly mixing waste powdered activated carbon with the mixed solution, cooling to room temperature, carrying out extrusion forming with hydraulic equipment, drying the formed carbon sample in a drying oven, carbonizing the dried formed carbon sample in a carbonization furnace at 500-800 DEG C, putting a right amount of carbonized sample in a rotary furnace, and activating at 700-900 DEG C by a water vapor activation process to obtain the final formed granular activated carbon. The method can prepare the formed granular activated carbon which has the characteristics of high strength, high caramel decolorization rate, high water resistance and the like.
Description
Technical field
The invention belongs to preparing technical field of the Sugarcane juice decolorization with shaped granule activated carbon, and in particular to one kind is using discarded
The method that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon.
Background technology
Activated carbon is widely used in the aspect such as the decolouring of gas phase and liquid phase, separation, refined.It is activated carbon for Sugarcane juice decolorization
One of main usess, the consumption of the kind activated carbon is big.Activated carbon for Sugarcane juice decolorization needs to be taken off with higher sugar liquid
Color rate, will reach higher Sugarcane juice decolorization rate, then require that activated carbon has more flourishing central hole structure, and in preparing have at present
The industrial process of the more flourishing activated carbon in hole is mainly the chemical activation methods such as phosphoric acid activation method and zinc chloride activation method, pollution
Than larger, clean manufacturing is difficult to realize.
At present, Activated carbon for refining of suger is mainly powdered activated carbon, and in actual use, powdered activated carbon is main
It is suitable for andnon-continuous operation manner, it is impossible to realize the continuous way operation of fixed bed.Shaped granule activated carbon can use fixed bed, have
Beneficial to realization continuous operation.Pressed active carbon is not required nothing more than with flourishing pore structure, higher absorption property, and is needed
There is enough intensity, during just can apply to actual continuous operation.At present, produce that pore structure is more flourishing and intensity compared with
High shaped granule activated carbon is mainly using chemical activation methods such as the physical activation methods such as steam activation, phosphoric acid although can produce
Go out shaped granule activated carbon, but its intensity is difficult to reach the use requirement of fixed bed.However, the work that vapor activation is produced
The pore-size of property charcoal is less, is generally in range of micropores, the activated carbon for industrially being produced with physical activation methods such as vapor
Generally there is no caramel decolorizing effect, that is, may not apply to caramel decolouring.Therefore, prepare and produce and decolourize with higher caramel
The higher shaped granule activated carbon of rate, intensity is a technical barrier in activated carbon field, is for a long time activated carbon academia
Research emphasis and industrial quarters research and development key areas.
Existing many patents disclose the preparation method of pressed active carbon, and patent (application number 200810055493.3) is announced
It is a kind of with coal dust as raw material, a kind of Colophonium is as adhesive and vapor is as activator column pressed active carbon production method,
Be mainly used in it is industrially desulfurized, based on microcellular structure, the not ability with Sugarcane juice decolorization.Patent (publication number CN1295027A) is public
A kind of pore structure regulation and control method of pressed active carbon of cloth.Its method is：The poly- second of pore creating material is added in raw material phenolic resin
Enol butyral and Polyethylene Glycol, in the supercritical state using steam activation, produce pressed active carbon.The method produces bar
Part requires that strictly cost is very high, and the activated carbon specific surface area and total pore volume of production are less, and pore structure is less flourishing, its ratio
Surface area is 1250m2.g-1, total pore volume is 0.67cm3.g-1.The method can increase the mesopore proportion of pressed active carbon, but
Sugarcane juice decolorization poor effect, not with using value.United States Patent (USP) US6787494 discloses a kind of manufacturer of pressed active carbon
Method.Its method is：Phenolic resin, water, methylcellulose, methanol mixed extrusion molding are added in powdery cocoanut active charcoal,
Pyrolysis is carried out under the conditions of 900 DEG C and obtains pressed active carbon.Intensity using the pressed active carbon prepared by the method is high, but hole
Structure is less flourishing, based on micropore, not with Sugarcane juice decolorization ability.
The content of the invention
Goal of the invention：For the deficiencies in the prior art, it is an object of the invention to provide a kind of using discarded powdery
The method that activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon, solve Sugarcane juice decolorization pressed active carbon have concurrently high intensity and
A production technology difficult problem for high Caramel adsorption, product have hole width it is larger, for characteristics such as Sugarcane juice decolorizations.
Technical scheme：In order to realize foregoing invention purpose, the technical solution used in the present invention is：
A kind of method for preparing Sugarcane juice decolorization shaped granule activated carbon using discarded powdered activated carbon, including following step
Suddenly：
(1) one or several in soluble starch, polyvinyl alcohol, polyvinyl butyral resin and Polyethylene Glycol are taken complete
Be dissolved in the water as additive, by additive and coal tar under conditions of heating mix homogeneously；
(2) in a heated condition, the additive in being crushed to the discarded powdered activated carbon of 100～200 purposes and step (1)
Mixing and stirring, wherein, it is 1 to discard powdered activated carbon with the mass ratio of coal tar:1～2.5, soluble starch, poly- second
The mass ratio of enol, polyvinyl butyral resin, one or several quality sums of Polyethylene Glycol and discarded powdered activated carbon
For 1:1～6；
(3) the mixing charcoal sample in step (2) is cooled to after room temperature and is squeezed under the pressure of 5～10t with hydraulic test
Type, and dry 12～48h is positioned in 100～150 DEG C of baking ovens；
(4) forming charcoal sample retort in step (3) is carried out carbonization under the conditions of 500～800 DEG C, is down to after room temperature and takes
To go out obtain carbonization sample；
(5) carbonization sample in step (4) is placed in living under the conditions of 700～900 DEG C using vapor activation in rotary furnace
Change, you can obtain final molding granular active carbon.
The discarded powdered activated carbon is Sugarcane juice decolorization and the applied field such as refined, wastewater treatment, monosodium glutamate decolourize, medicine is refined
Discarded powdered activated carbon after institute's use.
Described coal tar includes high temperature coal-tar, medium temperature coal tar and coalite tar.
Described discarded powdered activated carbon is ature of coal powdered activated carbon, shell powdered activated carbon or wooden powdered activated
Charcoal.
Charcoal sample extrusion molding under the pressure of 10t, is dried in 110～150 DEG C of baking ovens.
The charcoal sample retort that is dried in step (3) carries out carbonization at 800 DEG C.
Carbonization sample is placed in rotary furnace and is activated under the conditions of 850～900 DEG C using vapor activation.
Beneficial effect, compared with prior art, the present invention has advantages below：
1) raw material for producing shaped granule activated carbon is discarded powdered activated carbon, it is possible to achieve discarded powdered activated carbon is again
Utilize, reduce and waste and pollute, reduce production cost.
2) with the addition of in soluble starch, polyvinyl alcohol, polyvinyl butyral resin and Polyethylene Glycol in formative stage
Kind or several additives, product have hole width it is larger, for characteristics such as Sugarcane juice decolorizations.
3) effectively solving Sugarcane juice decolorization pressed active carbon has a production technology difficult problem for high intensity and high Caramel adsorption concurrently,
Effect is significant, the invention can prepare intensity height, water-tolerant, caramel decolorization rate can reach 110% high-performance sugar liquid
Decolouring pressed active carbon.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
20g soluble starches, 28g polyvinyl butyral resins, 14g polyethylene glycol 6000s such as are dissolved completely in into respectively at the quality
Deionized water in it is standby as additive, additive and 134g high temperature coal-tars are stirred under 80 DEG C of condition of water bath heating
Mixing, being subsequently adding the discarded coal mass active carbon 84g stirrings of 100 mesh drying more than half an hour makes to be sufficiently mixed uniformly, then will be upper
State mixture and pour mould into, column charcoal is squeezed under the pressure of 10t, the column charcoal for having extruded is put in 110 DEG C of baking oven
Be dried 24h, then take out to be down to room temperature and be put in retort and be heated to 800 DEG C with the heating rate of 5 DEG C/min, be incubated 2h charcoals
Room temperature taking-up is down to after change, above-mentioned carbonized material is placed in atmosphere swinging resistance furnace and is passed through nitrogen protection, with the liter of 5 DEG C/min
Warm speed is raised to 900 DEG C, simultaneously switches off nitrogen with the speed of 5mL/min and is passed through 150 DEG C, the vapor of 0.4MPa, after insulation 2h
Disconnect vapor and be passed through nitrogen and be down to after room temperature and pressed active carbon is obtained.Its performance is as shown in table 1.
Embodiment 2
14g polyvinyl alcohol, 7g Macrogol 4000s, 7g soluble starches are dissolved completely in etc. in quality deionized water and are made
It is standby for additive, additive and the stirring mixing of 67g high temperature coal-tars under 100 DEG C of condition of water bath heating, it is subsequently adding
The waste wood activated carbon 42g stirrings that are dried of 100 mesh more than half an hour make to be sufficiently mixed uniformly, then pour into said mixture
Mould, is squeezed into column charcoal under the pressure of 10t, the 48h that the is dried column charcoal for having extruded being put in 100 DEG C of baking oven, so
Take out afterwards to be down to room temperature and be put in retort and be heated to 800 DEG C with the heating rate of 10 DEG C/min, after insulation 2h carbonizations room is down to
Temperature is taken out, and above-mentioned carbonized material is placed in atmosphere swinging resistance furnace and is passed through nitrogen protection, is raised to the heating rate of 5 DEG C/min
, nitrogen being simultaneously switched off with the speed of 10mL/min and being passed through 130 DEG C, the vapor of 0.3MPa, after insulation 2h vapor is disconnected by 850 DEG C
It is passed through nitrogen and is down to after room temperature and pressed active carbon is obtained.Its performance is as shown in table 1.
Embodiment 3
By 20g polyvinyl butyral resins, 20g soluble starches, 10g polyethylene glycol 6000s be dissolved completely in etc. quality go from
It is standby as additive in sub- water, additive and the stirring mixing of 48g high temperature coal-tars under 80 DEG C of condition of water bath heating, so
Adding the waste wood activated carbon 30g stirrings of the drying of 100 mesh afterwards more than half an hour makes to be sufficiently mixed uniformly, then will be above-mentioned mixed
Compound pours mould into, and column charcoal is squeezed under the pressure of 10t, the column charcoal for having extruded is put into dry in 120 DEG C of baking oven
Dry 24h, then takes out to be down to room temperature and be put in retort and is heated to 800 DEG C, after insulation 2h carbonizations with the heating rate of 5 DEG C/min
Room temperature taking-up is down to, above-mentioned carbonized material is placed in atmosphere swinging resistance furnace and is passed through nitrogen protection, with the intensification speed of 5 DEG C/min
Rate is raised to 900 DEG C, simultaneously switches off nitrogen with the speed of 5mL/min and is passed through 150 DEG C, the vapor of 0.4MPa, disconnects after insulation 2h
Vapor is passed through nitrogen is down to after room temperature pressed active carbon is obtained.Its performance is as shown in table 1.
Comparative example 1
Waste wood activated carbon and 48g high-temperature coals are dried under 90 DEG C of condition of water bath heating what 30g was crushed to 100 mesh
Tar is mixed more than half an hour to be made to be sufficiently mixed uniformly, then pours said mixture into mould, is squeezed under the pressure of 10t
It is put into after molded in 100 DEG C of baking oven and is dried 48h, taking-up is down to after room temperature and is put in retort with the intensification speed of 10 DEG C/min
Rate is heated to 800 DEG C, and cooling after insulation 1h is taken out, and then above-mentioned carbonized material is placed in atmosphere swinging resistance furnace and is passed through nitrogen
Protection, while be raised to 900 DEG C with the heating rate of 10 DEG C/min, simultaneously switch off nitrogen with the speed of 5mL/min be passed through 150 DEG C,
The vapor of 0.4MPa, disconnects vapor and is passed through nitrogen and is down to after room temperature pressed active carbon is obtained after insulation 2h.Its performance
As shown in table 1.
Comparative example 2
The discarded cocoanut active charcoal of drying that 20g is crushed to 100 mesh is with 40g high temperature coal-tars in 80 DEG C of condition of water bath heating
Lower mixing more than half an hour makes to be sufficiently mixed uniformly, then pours said mixture into mould, extrudes under the pressure of 10t
It is put into after molding in 110 DEG C of baking oven and is dried 48h, taking-up is down to after room temperature and is put in retort with the heating rate of 10 DEG C/min
800 DEG C are heated to, cooling after insulation 2h is taken out, then above-mentioned carbonized material are placed in atmosphere swinging resistance furnace and are passed through nitrogen guarantor
Shield, while be raised to 850 DEG C with the heating rate of 10 DEG C/min, simultaneously switch off nitrogen with the speed of 5mL/min be passed through 150 DEG C,
The vapor of 0.4MPa, disconnects vapor and is passed through nitrogen and is down to after room temperature pressed active carbon is obtained after insulation 2h.Its performance
As shown in table 1.
Comparative example 3
The waste wood activated carbon that is dried that 30g is crushed to 100 mesh is mixed more than half an hour with 66g high temperature coal-tars
Make to be sufficiently mixed uniformly, then pour said mixture into mould, 120 DEG C of baking is put into after extrusion molding under the pressure of 10t
48h is dried in case, taking-up is down to after room temperature to be put in retort and is heated to 800 DEG C with the heating rate of 10 DEG C/min, is incubated 2h
Cooling afterwards is taken out, and then above-mentioned carbonized material is placed in atmosphere swinging resistance furnace and is passed through nitrogen protection, while with 10 DEG C/min
Heating rate be raised to 850 DEG C, simultaneously switch off nitrogen with the speed of 10mL/min and be passed through 150 DEG C, the vapor of 0.4MPa, insulation
Vapor is disconnected after 2h it is passed through nitrogen and is down to after room temperature and pressed active carbon is obtained.Its performance is as shown in table 1.
The performance parameter of each pressed active carbon in the embodiment of table 1 and comparative example
Note："/" is represented in table can not detect the value.
Claims (6)
1. it is a kind of to utilize the method that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon of discarding, it is characterised in that bag
Include following steps：
(1) one or several taken in soluble starch, polyvinyl alcohol, polyvinyl butyral resin and Polyethylene Glycol are completely dissolved
Yu Shuizhong as additive, by additive and coal tar under conditions of heating mix homogeneously；
(2) in a heated condition, mix with the additive in step (1) the discarded powdered activated carbon of 100～200 purposes is crushed to
Stir, wherein, it is 1 to discard powdered activated carbon with the mass ratio of coal tar:1～2.5, soluble starch, polyvinyl alcohol,
Polyvinyl butyral resin, one or several quality sums of Polyethylene Glycol are 1 with the mass ratio of discarded powdered activated carbon:1
～6；
(3) the mixing charcoal sample in step (2) is cooled to after room temperature and uses hydraulic test extrusion molding under the pressure of 5～10t, and
It is positioned in 100～150 DEG C of baking ovens and is dried 12～48h；
(4) forming charcoal sample retort in step (3) is carried out carbonization under the conditions of 500～800 DEG C, is down to after room temperature and takes out i.e.
Obtain carbonization sample；
(5) carbonization sample in step (4) is placed in rotary furnace and is activated under the conditions of 700～900 DEG C using vapor activation, i.e.,
Final molding granular active carbon is obtained；
The discarded powdered activated carbon is that Sugarcane juice decolorization is used with refined, wastewater treatment, monosodium glutamate decolouring, the refined application places of medicine
Discarded powdered activated carbon afterwards.
2. according to claim 1 utilization discards the side that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon
Method, it is characterised in that：Described coal tar includes high temperature coal-tar, medium temperature coal tar and coalite tar.
3. according to claim 1 utilization discards the side that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon
Method, it is characterised in that：Described discarded powdered activated carbon is ature of coal powdered activated carbon, shell powdered activated carbon or wooden powdery
Activated carbon.
4. according to claim 1 utilization discards the side that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon
Method, it is characterised in that：Charcoal sample extrusion molding under the pressure of 10t, is dried in 110～150 DEG C of baking ovens.
5. according to claim 1 utilization discards the side that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon
Method, it is characterised in that：The charcoal sample retort that is dried in step (3) carries out carbonization at 800 DEG C.
6. according to claim 1 utilization discards the side that powdered activated carbon prepares Sugarcane juice decolorization shaped granule activated carbon
Method, it is characterised in that：Carbonization sample is placed in rotary furnace and is activated under the conditions of 850～900 DEG C using vapor activation.
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| CN106865542A (en) * | 2017-02-23 | 2017-06-20 | 成都国化环保科技有限公司 | A kind of activated carbon with hollow morphology |
| CN107235489A (en) * | 2017-06-27 | 2017-10-10 | 南京林业大学 | A kind of preparation method of high-specific surface area Alveolate activated carbon |
| CN107185495A (en) * | 2017-07-05 | 2017-09-22 | 浙江省林业科学研究院 | The method and its activation equipment of a kind of useless burgy photo reversal type cellular activated carbon |
| CN108928972A (en) * | 2018-07-12 | 2018-12-04 | 李晓军 | Have effects that the bioactive water of lower hyperlipidemia, hypertension, hyperglycemia and its production technology |
| CN110357098A (en) * | 2019-07-10 | 2019-10-22 | 南京安捷特环保科技有限公司 | A kind of production method of active carbon by physical |
| CN110655077A (en) * | 2019-11-01 | 2020-01-07 | 海南星光活性炭有限公司 | Preparation method of coconut shell based columnar activated carbon |
| CN111573668B (en) * | 2020-05-22 | 2023-05-26 | 晋能控股煤业集团有限公司 | Activated carbon prepared from waste carbonized material powder, and preparation method and application thereof |
| CN115624952A (en) * | 2022-09-15 | 2023-01-20 | 城康材料技术有限公司 | Novel carbon material and preparation method and application thereof |
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| 成型活性炭制备技术研究进展;闫新龙等;《化工进展》;20081231;第27卷(第12期);1868－1881 * |
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