CN115818642B - Production method of self-adhesive high-strength wood columnar activated carbon - Google Patents
Production method of self-adhesive high-strength wood columnar activated carbon Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 239000002023 wood Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 239000000853 adhesive Substances 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 135
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 119
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 106
- 238000005406 washing Methods 0.000 claims abstract description 65
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 53
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 239000002028 Biomass Substances 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 24
- 230000003213 activating effect Effects 0.000 claims abstract description 18
- 238000005469 granulation Methods 0.000 claims abstract description 10
- 230000003179 granulation Effects 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 34
- 239000011265 semifinished product Substances 0.000 claims description 23
- 238000004898 kneading Methods 0.000 claims description 22
- 238000007599 discharging Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- 239000000428 dust Substances 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 238000013007 heat curing Methods 0.000 claims description 14
- 239000005539 carbonized material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000004615 ingredient Substances 0.000 claims description 12
- 238000001125 extrusion Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000009656 pre-carbonization Methods 0.000 claims description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 8
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 8
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 8
- 241001330002 Bambuseae Species 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 8
- 239000011425 bamboo Substances 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 238000002485 combustion reaction Methods 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 239000003546 flue gas Substances 0.000 claims description 8
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 239000003456 ion exchange resin Substances 0.000 claims description 8
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 8
- 239000003345 natural gas Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 10
- 238000001029 thermal curing Methods 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 229910019142 PO4 Inorganic materials 0.000 abstract description 2
- 239000010452 phosphate Substances 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000009467 reduction Effects 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 239000007789 gas Substances 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 235000013399 edible fruits Nutrition 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 235000012343 cottonseed oil Nutrition 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Abstract
The invention discloses a production method of self-adhesive high-strength wood column-shaped active carbon, which belongs to the technical field of active carbon adsorption material production, wherein the column-shaped active carbon is produced by a phosphoric acid method, biomass and phosphoric acid are mixed and carbonized and then granulated, the size uncertainty shrinkage after material granulation is reduced, the shape and the size of the material are stable, residual phosphate of the column-shaped active carbon which is not completely washed and functional groups on the surface of the carbon are subjected to high-temperature thermal curing polycondensation modification through the thermocuring of an anoxic micro-negative pressure environment, and the strength and the stacking density of the column-shaped active carbon are improved; the phosphoric acid recovery replaces the traditional gradient recovery method of transition in the gradient acid tank by adopting the gradient recovery method of directly and serially filling the water washing tanks with the activating materials, thereby improving the phosphoric acid recovery efficiency, reducing the hot water consumption for extraction, increasing the phosphoric acid recovery concentration and realizing energy conservation and consumption reduction. The invention also has the advantages of simple process, high automation degree, high production efficiency and the like, and is favorable for industrialized popularization and application.
Description
Technical Field
The invention belongs to the technical field of active carbon adsorption material production, and particularly relates to a production method of self-adhesive high-strength wood columnar active carbon.
Background
Most of common columnar activated carbon is physically coal-based activated carbon, which is mainly prepared by adding binders such as coal tar, asphalt and the like into pulverized coal, extruding, forming and granulating, and then physically activating the activated carbon. The physical method coal-based activated carbon product has high strength and high specific gravity, but has lower adsorption performance due to the limitation of physical method activation. The wood columnar carbon is prepared by mixing biomass powder with phosphoric acid, kneading, forming and granulating, and activating the carbon, and has the defects of high adsorption performance, low strength and low specific gravity. The wood columnar activated carbon with high strength, high specific gravity and high adsorption performance is less in the market, and the production cost is higher.
The application number is CN201110144557.9, the method for preparing the solvent recovery activated carbon by using the wood material and the method for preparing the solvent recovery activated carbon by using the wood chip as the raw material are disclosed, and the application number is CN201210097738.5, wherein the catalyst adopted by the two technologies is phosphoric acid, and inorganic salts such as zinc chloride, calcium chloride, sulfuric acid, boric acid, potassium dichromate, potassium permanganate and disodium hydrogen phosphate are also added, so that metal ions are continuously enriched, the purity of phosphoric acid in a system is continuously reduced, and high-efficiency catalytic pore-forming is difficult to realize. The application number is CN201710531774.0, the wood particle activated carbon for the automobile carbon tank and the preparation method thereof adopt the primary activation by the phosphoric acid method and the secondary activation by the physical method, the production process is more complex, the cost is higher, and the ash content of the product is higher due to the adoption of the inorganic binder, so that the wood columnar activated carbon with high adsorption is difficult to obtain.
Disclosure of Invention
The invention aims to provide a production method of self-adhesive high-strength wood columnar activated carbon, so as to solve the problems.
In order to solve the technical problems, the invention adopts the following technical scheme:
the production method of the self-adhesive high-strength wood columnar activated carbon comprises the following steps:
1) Pretreatment of raw materials: drying, crushing, desanding and deironing the three residues of the biomass to obtain biomass powder;
2) Kneading ingredients: feeding the biomass powder obtained in the step 1) and the circulating acid into a kneader with a hot water jacket for kneading to obtain a kneaded material;
3) Pre-carbonizing: conveying the kneaded material in the step 2) to an internal heating rotary furnace for dehydration and pre-carbonization to obtain a pre-carbonized material;
4) Refining into mud: conveying the pre-carbonized material in the step 3) to a vacuumizing extruder for extrusion molding to obtain refined columnar pug;
5) And (3) mold forming: conveying the refined columnar pug obtained in the step 4) to an extruder provided with a columnar die for granulation, and then automatically cutting to obtain granular columnar wet materials;
6) And (5) drying and forming: drying the granular columnar wet material obtained in the step 5) to obtain columnar dry material;
7) Activating: conveying the columnar dry material in the step 6) to a 400-500 ℃ anoxic micro negative pressure internal heating rotary furnace through a sealing feeder for activation for 1-4 hours, and then cooling and discharging to obtain columnar activated material;
8) Recovery and washing: conveying the columnar activated material in the step 7) to a water washing tank to sequentially perform phosphoric acid gradient recovery and hot water washing to obtain columnar activated carbon washing incomplete material;
9) And (5) filtering and drying: discharging the cylindrical active carbon washing incomplete material obtained in the step 8) from the bottom of a water washing tank, filtering water by a mesh belt, absorbing water and drying to obtain a cylindrical active carbon semi-finished product;
10 Heat curing): and (3) putting the columnar activated carbon semi-finished product obtained in the step (9) into an anoxic micro negative pressure external heating rotary furnace at 500-800 ℃ for heat curing for 0.5-3 hours, obtaining hot air through a heat exchanger by using heat cured flue gas, heating and drying, and then indirectly cooling and cooling the discharged material to obtain the high-strength wood columnar activated carbon.
Further, in the step 1), the biomass powder is selected from any one or more of wood dust powder, bamboo dust powder, cotton seed powder and shell powder; the granularity is within 10% of the passing rate of 200 meshes and 95% of water.
Further, in the step 2), the mass ratio of the biomass powder to the circulating acid is 1:2-3; the temperature of the hot water jacket is 80-100 ℃; kneading time is 20-40 min; the circulating acid is 55-65% phosphoric acid.
Further, in the step 3), the heat source of the internal heating rotary furnace is hot air provided by natural gas combustion, and the temperature is kept to form a thick protective atmosphere of carbon dioxide and nitrogen; the temperature of the internal heating rotary furnace is 120-160 ℃, and the pre-carbonization time is 0.5-2h.
Further, in the step 4), a spiral mud refining machine is adopted as the extruder, and cylindrical refined mud materials with the diameter of 10-40mm are extruded by the spiral mud refining machine; the pressure value of the vacuumizing is-0.06 to-0.09 MPa.
Further, in the step 5), the extruder with the columnar die adopts a spiral extrusion granulator, the granulation diameter is 2-8mm, and a discharge hole of the granulator is provided with a rotary cutter head for automatic cutting.
Further, in the step 6), a multi-layer mesh belt dryer is adopted to gradually dry the materials at the temperature of 80-180 ℃ in sequence, and the moisture after drying is within 5%; and the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Preferably, the recovery washing in step 8) is specifically: adopting water washing tanks with the height-diameter ratio of more than 3 and provided with a filter screen layer, connecting more than 6 water washing tanks filled with activated materials in series for gradient recovery of phosphoric acid and gradient washing, wherein the running route of the activated materials is opposite to that of hot water, feeding hot water into the tank 1, discharging gradient phosphoric acid from the tank at the tail of the tank, purifying the obtained gradient phosphoric acid by adopting ion exchange resin, and recycling the purified gradient phosphoric acid for kneading ingredients in the step 2); the step 9) of water filtration and drying is specifically as follows: the pump circulation flushing is adopted to discharge from the bottom of the water washing tank, the materials are sent to a dryer through a filter screen conveyer belt with a water absorbing device, and the water content after drying is within 5%, so that a columnar active carbon semi-finished product is obtained.
Further, the pH of the cylindrical active carbon washing incomplete material in the step 8) is 1.8-3.
Further, the micro negative pressure in the step 3), the step 7) and the step 10) is between-5 pa and-200 pa.
The invention has the following advantages:
1) According to the invention, the wood column-shaped active carbon is produced by adopting a phosphoric acid method, and the ingredients are mixed and then pre-carbonized and granulated, so that the material is stable in form and size, high in strength and self-adhesive property, and the granulated product is uniform, and meanwhile, the pre-carbonized product has a certain dehydration effect, so that the activation pore-forming effect is enhanced, and meanwhile, the productivity is improved.
2) The invention adopts the heat curing in the anoxic micro-negative pressure environment, and the columnar activated carbon is not completely washed, and the residual phosphate and the carbon surface functional groups are subjected to high-temperature heat curing polycondensation modification, so that the strength and the bulk density of the columnar activated carbon are improved.
3) According to the invention, the tanks filled with the activating materials in series are adopted to perform heat energy gradient recovery and phosphoric acid purification and concentration, the running route of the activating materials is opposite to that of hot water, hot water is fed into the series 1 tank, gradient phosphoric acid is discharged from the series tail tank, the traditional phosphoric acid recovery and washing modes of the gradient phosphoric acid tank and the gradient water are replaced, the efficient comprehensive utilization of heat energy is maintained, and the unit energy consumption and acid consumption are reduced.
4) The invention has simple production process, high automation degree and high production efficiency, and is beneficial to industrialized popularization.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the invention provides a production method of self-adhesive high-strength wood columnar activated carbon, which comprises the following steps:
1) Pretreatment of raw materials: drying, crushing, desanding and deironing the three residues of the biomass to obtain biomass powder with the passing rate of 200 meshes of 90% and the moisture of 10%; wherein the biomass powder is selected from one or more of wood dust powder, bamboo dust powder, cotton seed powder and shell powder.
2) Kneading ingredients: and (2) adding the biomass powder obtained in the step (1) and 55-65% of circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:2-3, and kneading for 20-40 min to obtain a kneaded material.
3) Pre-carbonizing: conveying the kneaded material in the step 2) to 120-160 ℃ through a conveying belt, and dehydrating and pre-carbonizing the kneaded material in a micro negative pressure internal heating rotary furnace of-5 to-200 pa for 0.5-2h to obtain a pre-carbonized material; the heat source of the internal heating rotary furnace is hot air provided by natural gas combustion, and the internal heating rotary furnace maintains the temperature and forms a thick protective atmosphere of carbon dioxide and nitrogen.
4) Refining into mud: conveying the pre-carbonized material in the step 3) to a spiral mud mill vacuumized under the pressure of minus 0.06 to minus 0.09MPa through a conveying belt, extruding the pre-carbonized material into columnar refined mud with the diameter of 10-40mm, and obtaining refined columnar mud;
5) And (3) mold forming: conveying the refined columnar pug obtained in the step 4) to an extruder with a columnar die through a conveying belt for extrusion molding and granulation, wherein the extruder with the columnar die adopts a spiral extrusion granulator, the granulation diameter is 2-8mm, and a discharge port of the granulator is provided with a rotary cutter head for automatic cutting to obtain granular columnar wet materials;
6) And (5) drying and forming: conveying the granular columnar wet materials obtained in the step 5) to a multi-layer mesh belt dryer through a conveying belt, and then gradually drying at a temperature of 80-180 ℃ in sequence, wherein the moisture content after drying is within 5%, so as to obtain columnar dry materials; and the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
7) Activating: conveying the columnar dry material in the step 6) to a 400-500 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 1-4 hours, and cooling and discharging to obtain columnar activated material;
8) Recovery and washing: conveying the columnar activated material in the step 7) to a water washing tank to sequentially perform phosphoric acid gradient recovery and hot water washing to obtain columnar activated carbon washing incomplete material; the method specifically comprises the steps of adopting a water washing tank with an aspect ratio of more than 3 and a filter screen layer, connecting more than 6 water washing tanks filled with activating materials in series to perform gradient recovery phosphoric acid and gradient washing, enabling the running route of the activating materials to be opposite to that of hot water, feeding hot water into a tank 1, discharging gradient phosphoric acid from a tank tail part of the tank, purifying the obtained gradient phosphoric acid by adopting ion exchange resin, and recycling the purified gradient phosphoric acid for kneading ingredients in the step 2); the pH value of the columnar active carbon washing incomplete material is 1.8-3.
9) And (5) filtering and drying: discharging the incomplete material washed by the columnar activated carbon in the step 8) from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan and absorbs water on the surface of the material.
10 Heat curing): putting the columnar active carbon semi-finished product obtained in the step 9) into an anoxic micro negative pressure external heating rotary furnace at 500-800 ℃ and 5-200 pa for heat curing for 0.5-3 h, wherein the heat curing is used for enhancing the strength, and simultaneously adjusting the surface functional groups to improve the chemical adsorption performance and reduce the impurity of the product. And (3) hot air is obtained from the heat-cured flue gas through a heat exchanger and is used for heating and drying, and then the discharged material is indirectly cooled and cooled to obtain the high-strength wood columnar activated carbon.
Example 1
Drying, crushing, desanding and deironing wood dust, bamboo dust, fruit shells and cotton seeds to obtain biomass powder with a passing rate of 90% and moisture content of 10% of 200 meshes, adding the biomass powder and 55% of circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:2, kneading for 20min, conveying the kneaded materials to a 120 ℃ and-5 to-200 pa micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization for 2h, wherein an internal heating source is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a spiral mud-smelting machine vacuumized under the pressure of minus 0.06 to minus 0.09MPa to extrude into columnar refined mud with the diameter of 10-40mm, granulating the refined columnar mud by a spiral extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge port of the granulator by a rotary cutter disc to obtain granular columnar wet materials; the granular columnar wet materials are conveyed to a multi-layer mesh belt dryer, and are gradually dried in a temperature section of 80-180 ℃ in sequence, and the moisture content after drying is controlled within 5% to obtain columnar dry materials; wherein, the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Conveying the columnar dry material to a 400 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 4 hours, and cooling and discharging to obtain columnar activated material; the columnar activated material adopts a water washing tank with the height-diameter ratio of more than 3 and a filter screen layer, more than 6 water washing tanks filled with the activated material are connected in series to carry out gradient recovery phosphoric acid and gradient washing, the running route of the activated material is opposite to that of hot water, 1 tank is connected in series to feed hot water, the tail tank is connected with the gradient phosphoric acid, the obtained gradient phosphoric acid is purified by adopting ion exchange resin and then is recycled for kneading ingredients, and the pH value of the obtained columnar activated carbon washing incomplete material is 3; discharging the incomplete material washed by the columnar activated carbon from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan, water on the surface of a material is absorbed to be dry, a columnar active carbon semi-finished product is put into a 800 ℃ to-5 to-200 pa anoxic micro negative pressure external heating type rotary furnace for thermal curing for 3 hours, hot air is obtained from heat-cured flue gas through a heat exchanger for heating and drying, and then the material is discharged, cooled and cooled indirectly to obtain the high-strength wooden columnar active carbon.
Example 2
Drying, crushing, desanding and deironing wood dust, bamboo dust, fruit shells and cotton seeds to obtain biomass powder with a passing rate of 90% and moisture content of 10% of 200 meshes, adding the biomass powder and 55% of circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:2, kneading for 20min, conveying the kneaded materials to a 120 ℃ and-5 to-200 pa micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization for 2h, wherein an internal heating source is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a spiral mud-smelting machine vacuumized under the pressure of minus 0.06 to minus 0.09MPa to extrude into columnar refined mud with the diameter of 10-40mm, granulating the refined columnar mud by a spiral extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge port of the granulator by a rotary cutter disc to obtain granular columnar wet materials; the granular columnar wet materials are conveyed to a multi-layer mesh belt dryer, and are gradually dried in a temperature section of 80-180 ℃ in sequence, and the moisture content after drying is controlled within 5% to obtain columnar dry materials; wherein, the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Conveying the columnar dry material to a 400 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 4 hours, and cooling and discharging to obtain columnar activated material; the columnar activated material adopts a water washing tank with the height-diameter ratio of more than 3 and a filter screen layer, more than 6 water washing tanks filled with the activated material are connected in series to carry out gradient recovery phosphoric acid and gradient washing, the running route of the activated material is opposite to that of hot water, 1 tank is connected in series, the tail of the string is connected with gradient phosphoric acid, the obtained gradient phosphoric acid is purified by adopting ion exchange resin and then is recycled for kneading ingredients, and the pH value of the obtained columnar activated carbon washing incomplete material is 1.8; discharging the incomplete material washed by the columnar activated carbon from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan, water on the surface of a material is absorbed to be dry, a columnar active carbon semi-finished product is put into a 500 ℃ to-5 to-200 pa anoxic micro negative pressure external heating type rotary furnace for thermal curing for 3 hours, hot air is obtained from heat-cured flue gas through a heat exchanger for heating and drying, and then the material is discharged, cooled and cooled indirectly to obtain the high-strength wooden columnar active carbon.
Example 3
Drying, crushing, desanding and deironing wood dust, bamboo dust and fruit shells to obtain biomass powder with a 200-mesh passing rate of 90% and a water content of 10%, adding the biomass powder and 60% circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:3, kneading for 30min, conveying the kneaded materials to a 130 ℃ and-5 to-200 pa micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization for 1.5h, wherein an internal heating source is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a spiral mud-smelting machine vacuumized under the pressure of minus 0.06 to minus 0.09MPa to extrude into columnar refined mud with the diameter of 10-40mm, granulating the refined columnar mud by a spiral extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge port of the granulator by a rotary cutter disc to obtain granular columnar wet materials; the granular columnar wet materials are conveyed to a multi-layer mesh belt dryer, and are gradually dried in a temperature section of 80-180 ℃ in sequence, and the moisture content after drying is controlled within 5% to obtain columnar dry materials; wherein, the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Conveying the columnar dry material to a 450 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 2 hours, and cooling and discharging to obtain columnar activated material; the columnar activated material adopts a water washing tank with the height-diameter ratio of more than 3 and a filter screen layer, more than 6 water washing tanks filled with the activated material are connected in series to carry out gradient recovery phosphoric acid and gradient washing, the running route of the activated material is opposite to that of hot water, 1 tank is connected in series to feed hot water, the tail tank is connected with the gradient phosphoric acid, the obtained gradient phosphoric acid is purified by adopting ion exchange resin and then is recycled for kneading ingredients, and the pH value of the obtained columnar activated carbon washing incomplete material is 3; discharging the incomplete material washed by the columnar activated carbon from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan, water on the surface of a material is absorbed to be dry, a columnar active carbon semi-finished product is put into a 600 ℃, -5-200 pa anoxic micro negative pressure external heating rotary furnace for thermal curing for 2 hours, hot air is obtained from heat-cured flue gas through a heat exchanger for heating and drying, and then the material is discharged, cooled indirectly and cooled to obtain the high-strength wooden columnar active carbon.
Example 4
Drying, crushing, desanding and deironing wood dust, bamboo dust, fruit shells and cotton seeds to obtain biomass powder with a 200-mesh passing rate of 90% and a water content of 10%, adding the biomass powder and 65% circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:2.5, kneading for 40min, conveying the kneaded material to a 145 ℃ and-5 to-200 pa micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization for 1h, wherein an internal heating source is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a spiral mud-smelting machine vacuumized under the pressure of minus 0.06 to minus 0.09MPa to extrude into columnar refined mud with the diameter of 10-40mm, granulating the refined columnar mud by a spiral extrusion granulator with the granulating diameter of 2-8mm, and automatically cutting a discharge port of the granulator by a rotary cutter disc to obtain granular columnar wet materials; the granular columnar wet materials are conveyed to a multi-layer mesh belt dryer, and are gradually dried in a temperature section of 80-180 ℃ in sequence, and the moisture content after drying is controlled within 5% to obtain columnar dry materials; wherein, the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Conveying the columnar dry material to a 480 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 1h, and cooling and discharging to obtain columnar activated material; the columnar activated material adopts a water washing tank with the height-diameter ratio of more than 3 and a filter screen layer, more than 6 water washing tanks filled with the activated material are connected in series to carry out gradient recovery phosphoric acid and gradient washing, the running route of the activated material is opposite to that of hot water, 1 tank is connected in series, the tail of the string is connected with gradient phosphoric acid, the obtained gradient phosphoric acid is purified by adopting ion exchange resin and then is recycled for kneading ingredients, and the pH value of the obtained columnar activated carbon washing incomplete material is 2.8; discharging the incomplete material washed by the columnar activated carbon from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan, water on the surface of a material is absorbed to be dry, a columnar active carbon semi-finished product is put into a 700 ℃, -5-200 pa anoxic micro negative pressure external heating rotary furnace for thermal curing for 1h, hot air is obtained from heat-cured flue gas through a heat exchanger for heating and drying, and then the material is discharged, cooled indirectly and cooled to obtain the high-strength wooden columnar active carbon.
Example 5
Drying, crushing, desanding and deironing wood dust, bamboo dust and fruit shells to obtain biomass powder with a 200-mesh passing rate of 90% and a moisture of 10%, adding the biomass powder and 55% circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to a mass ratio of 1:3, kneading for 30min, conveying the kneaded materials to a 160 ℃ and-5 to-200 pa micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization for 0.5h, wherein an internal heating source is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a spiral mud-smelting machine vacuumized under the pressure of minus 0.06 to minus 0.09MPa to extrude into columnar refined mud with the diameter of 10-40mm, granulating the refined columnar mud by a spiral extrusion granulator with the granulating diameter of 2-8mm, and automatically cutting a discharge port of the granulator by a rotary cutter disc to obtain granular columnar wet materials; the granular columnar wet materials are conveyed to a multi-layer mesh belt dryer, and are gradually dried in a temperature section of 80-180 ℃ in sequence, and the moisture content after drying is controlled within 5% to obtain columnar dry materials; wherein, the dry tail gas is recycled by a spray tower to obtain a large amount of hot water, and the hot water is recycled for production.
Conveying the columnar dry material to a 500 ℃ and-5 to-200 pa anoxic micro negative pressure internal heating rotary furnace through a sealing feeder, activating for 4 hours, and cooling and discharging to obtain columnar activated material; the columnar activated material adopts a water washing tank with the height-diameter ratio of more than 3 and a filter screen layer, more than 6 water washing tanks filled with the activated material are connected in series to carry out gradient recovery phosphoric acid and gradient washing, the running route of the activated material is opposite to that of hot water, 1 tank is connected in series, the tail of the string is connected with gradient phosphoric acid, the obtained gradient phosphoric acid is purified by adopting ion exchange resin and then is recycled for kneading ingredients, and the pH value of the obtained columnar activated carbon washing incomplete material is 2.5; discharging the incomplete material washed by the columnar activated carbon from the bottom of a water washing tank by adopting pump circulation flushing, and conveying the material to a dryer through a filter screen conveying belt with a water absorbing device, wherein the water content after drying is within 5%, so as to obtain a columnar activated carbon semi-finished product; the water absorbing device consists of a water absorbing disc, a cyclone separator and a high-pressure fan, water on the surface of a material is absorbed to be dry, a columnar active carbon semi-finished product is put into a 800 ℃ to-5 to-200 pa anoxic micro negative pressure external heating type rotary furnace for thermal curing for 0.5h, hot air is obtained from heat-cured flue gas through a heat exchanger and used for heating and drying, and then the material is discharged and cooled indirectly to obtain the high-strength wood columnar active carbon.
Comparative example 1
The technical scheme of this comparative example is basically the same as that of example 1, except that the pH of the post-washing column-shaped activated carbon incompletely washed material is 1.5.
Comparative example 2
The technical scheme of this comparative example is basically the same as that of example 1, except that the pH of the post-washing column-shaped activated carbon incompletely washed material is 1.0.
Comparative example 3
The technical scheme of this comparative example is basically the same as that of example 1, except that the pH of the post-washing column-shaped activated carbon incompletely washed material is 3.5.
Comparative example 4
The technical scheme of this comparative example is basically the same as that of example 1, except that the pH of the post-washing column-shaped activated carbon incompletely washed material is 4.0.
Comparative example 5
The technical scheme of this comparative example is basically the same as that of example 5, except that the heat curing temperature of the columnar activated carbon semi-finished product is 900 ℃.
Comparative example 6
The technical scheme of this comparative example is basically the same as that of example 5, except that the heat curing temperature of the columnar activated carbon semi-finished product is 850 ℃.
Comparative example 7
The technical scheme of this comparative example is basically the same as that of example 5, except that the heat curing temperature of the columnar activated carbon semi-finished product is 450 ℃.
Comparative example 8
The technical scheme of this comparative example is basically the same as that of example 5, except that the heat curing temperature of the columnar activated carbon semi-finished product is 400 ℃.
Product performance detection
The adsorption performance, particle and other indexes of the activated carbon prepared in examples 1 to 5 and comparative examples 1 to 8 were respectively tested, and the test results are shown in the following table:
intensity test reference: determination of the intensity of the GB/T12496.6-1999 woody activated carbon test method
From the above data, it can be seen that the adsorption performance and strength of the columnar activated carbon prepared in examples 1-5 of the present invention are better than those of the columnar activated carbon sold in the market, i.e. the columnar activated carbon prepared in the present invention has higher strength and better adsorption performance.
As can be seen from the data of comparative examples 1-2 and comparative examples 1-4, when the pH of the post-activated carbon washed incomplete charge is too low, the adsorption value decreases and ash increases. Comparative examples 3-4 it can be seen that the strength of the columnar activated carbon tends to decrease when the pH of the incompletely washed columnar activated carbon is too high. Therefore, according to experimental data, when the pH of the columnar active carbon washing incomplete material is 1.8-3, the prepared active carbon has better strength and adsorption performance, and the ash content is lower.
The data of comparative example 5 and comparative examples 5 to 8 show that the activated carbon adsorption performance generally decreases as the thermosetting temperature of the columnar activated carbon semi-finished product increases. When the temperature is lower than 500 ℃, the strength of the activated carbon tends to decrease, and ash increases. The heat curing temperature is 500-800 ℃ according to the invention by comprehensively considering the energy consumption, the strength of the activated carbon and the adsorption performance.
While the foregoing is directed to embodiments, embodiments and advantages of the present invention, other and further details of the invention may be had by the foregoing description, it should be understood that the invention is not limited to the particular embodiments and embodiments disclosed, but is intended to cover all modifications, equivalents, alternatives, and modifications falling within the spirit and principles of the invention.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The production method of the self-adhesive high-strength wood columnar activated carbon is characterized by comprising the following steps of:
1) Pretreatment of raw materials: drying, crushing, desanding and deironing the three residues of the biomass to obtain biomass powder; the biomass powder is selected from any one or more of wood dust powder, bamboo dust powder, cotton seed powder and shell powder; the granularity is more than 95% of the passing rate of 200 meshes, and the moisture is within 10%;
2) Kneading ingredients: feeding the biomass powder obtained in the step 1) and the circulating acid into a kneader with a hot water jacket for kneading to obtain a kneaded material; wherein the mass ratio of the biomass powder to the circulating acid is 1:2-3; the temperature of the hot water jacket is 80-100 ℃; kneading time is 20-40 min; the circulating acid is 55-65% phosphoric acid;
3) Pre-carbonizing: conveying the kneaded material in the step 2) to a micro negative pressure internal heating rotary furnace for dehydration and pre-carbonization to obtain a pre-carbonized material; the heat source of the internal heating rotary furnace is hot air provided by natural gas combustion, and the temperature is kept to form a thick carbon dioxide and nitrogen protective atmosphere; the temperature of the internal heating rotary furnace is 120-160 ℃, and the pre-carbonization time is 0.5-2h;
4) Refining into mud: conveying the pre-carbonized material in the step 3) to a vacuumizing extruder for extrusion molding to obtain refined columnar pug;
5) And (3) mold forming: conveying the refined columnar pug obtained in the step 4) to an extruder provided with a columnar die for granulation, and then automatically cutting to obtain granular columnar wet materials;
6) And (5) drying and forming: drying the granular columnar wet material obtained in the step 5) to obtain columnar dry material;
7) Activating: conveying the columnar dry material in the step 6) to a 400-500 ℃ anoxic micro negative pressure internal heating rotary furnace through a sealing feeder for activation for 1-4 hours, and then cooling and discharging to obtain columnar activated material;
8) And (3) recovering and washing in series: conveying the columnar activated material in the step 7) to a water washing tank connected in series to sequentially perform phosphoric acid gradient recovery and hot water washing, wherein the running route of the activated material is opposite to that of the hot water, hot water is fed into the tank 1, and gradient phosphoric acid is discharged from the tank tail part of the tank 1, so that a columnar activated carbon washing incomplete material is obtained; the pH value of the columnar active carbon washing incomplete material is 1.8-3;
9) And (5) filtering and drying: discharging the cylindrical active carbon washing incomplete material obtained in the step 8) from the bottom of a water washing tank, filtering water by a mesh belt, absorbing water and drying to obtain a cylindrical active carbon semi-finished product;
10 Heat curing): and (3) putting the columnar activated carbon semi-finished product obtained in the step (9) into an anoxic micro negative pressure external heating rotary furnace at 500-800 ℃ for heat curing for 0.5-3 hours, obtaining hot air through a heat exchanger by using heat cured flue gas, heating and drying, and then indirectly cooling and cooling the discharged material to obtain the high-strength wood columnar activated carbon.
2. The method for producing the self-adhesive high-strength wood columnar activated carbon according to claim 1, wherein in the step 4), a spiral mud refining machine is adopted as the extruder, and columnar refined mud materials with the diameter of 10-40mm are extruded by the spiral mud refining machine; the pressure value of the vacuumizing is-0.06 to-0.09 MPa.
3. The method for producing the self-adhesive high-strength wood columnar activated carbon according to claim 1, wherein in the step 5), an extruder with a columnar die is selected from a spiral extrusion granulator, the granulation diameter is 2-8mm, and a discharge hole of the granulator is provided with a rotary cutter for automatic cutting.
4. The method for producing the self-adhesive high-strength wood columnar active carbon according to claim 1, wherein in the step 6), a multi-layer mesh belt dryer is adopted to gradually dry the active carbon at a temperature of 80-180 ℃ in sequence, and the moisture after drying is within 5%.
5. The method for producing self-adhesive high-strength wood columnar activated carbon according to claim 1, wherein the recovery washing in step 8) is specifically: adopting water washing tanks with the height-diameter ratio of more than 3 and provided with a filter screen layer, connecting more than 6 water washing tanks filled with activating materials in series to perform gradient recovery phosphoric acid and gradient washing, wherein the running route of the activating materials is opposite to that of hot water, feeding hot water into the tank 1, discharging gradient phosphoric acid from the tank at the tail of the tank, purifying the obtained gradient phosphoric acid by adopting ion exchange resin, and recycling the purified gradient phosphoric acid for kneading ingredients in the step 2); the step 9) of water filtration and drying is specifically as follows: the pump circulation flushing is adopted to discharge from the bottom of the water washing tank, the materials are sent to a dryer through a filter screen conveyer belt with a water absorbing device, and the water content after drying is within 5%, so that a columnar active carbon semi-finished product is obtained.
6. The method for producing self-adhesive high-strength wood columnar activated carbon according to claim 1, wherein the micro negative pressure in step 3), step 7) and step 10) is-5 to-200 Pa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102247806A (en) * | 2011-05-31 | 2011-11-23 | 福建省鑫森炭业股份有限公司 | Activated carbon for solvent recovery produced from wood materials and preparation method thereof |
| CN102698724A (en) * | 2012-04-06 | 2012-10-03 | 淮北市大华活性炭有限公司 | Method for producing active carbon for gasoline vapor adsorption |
| CN106348264A (en) * | 2016-09-29 | 2017-01-25 | 浙江省林业科学研究院 | Device for countercurrent recovering phosphoric acid from chemical activation material |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247806A (en) * | 2011-05-31 | 2011-11-23 | 福建省鑫森炭业股份有限公司 | Activated carbon for solvent recovery produced from wood materials and preparation method thereof |
| CN102698724A (en) * | 2012-04-06 | 2012-10-03 | 淮北市大华活性炭有限公司 | Method for producing active carbon for gasoline vapor adsorption |
| CN106348264A (en) * | 2016-09-29 | 2017-01-25 | 浙江省林业科学研究院 | Device for countercurrent recovering phosphoric acid from chemical activation material |
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