CN115818642A - Production method of self-bonding high-strength wood columnar activated carbon - Google Patents
Production method of self-bonding high-strength wood columnar activated carbon Download PDFInfo
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- CN115818642A CN115818642A CN202211582283.6A CN202211582283A CN115818642A CN 115818642 A CN115818642 A CN 115818642A CN 202211582283 A CN202211582283 A CN 202211582283A CN 115818642 A CN115818642 A CN 115818642A
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- phosphoric acid
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 199
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 239000002023 wood Substances 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 135
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 117
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 102
- 238000005406 washing Methods 0.000 claims abstract description 58
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 51
- 239000002028 Biomass Substances 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 19
- 238000001029 thermal curing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 10
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- 239000002253 acid Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 62
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 35
- 238000004898 kneading Methods 0.000 claims description 24
- 238000007599 discharging Methods 0.000 claims description 21
- 239000011265 semifinished product Substances 0.000 claims description 21
- 238000010521 absorption reaction Methods 0.000 claims description 20
- 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
- 239000005539 carbonized material Substances 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 11
- 238000010000 carbonizing Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 10
- 229920001187 thermosetting polymer Polymers 0.000 claims description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 9
- 239000003546 flue gas Substances 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
- 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
- 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
- 235000013399 edible fruits Nutrition 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009656 pre-carbonization Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 241001408630 Chloroclystis Species 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 4
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- 125000000524 functional group Chemical group 0.000 abstract description 3
- 229910019142 PO4 Inorganic materials 0.000 abstract description 2
- 230000009286 beneficial effect Effects 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
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- 238000004134 energy conservation Methods 0.000 abstract 1
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- 230000000052 comparative effect Effects 0.000 description 21
- 239000004615 ingredient Substances 0.000 description 9
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- 238000002485 combustion reaction Methods 0.000 description 7
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- 239000007921 spray Substances 0.000 description 7
- 239000002918 waste heat Substances 0.000 description 7
- 238000000053 physical method Methods 0.000 description 5
- 235000012343 cottonseed oil Nutrition 0.000 description 4
- 238000013007 heat curing Methods 0.000 description 4
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- 230000007423 decrease Effects 0.000 description 3
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- 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
- 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
- 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
- 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
- 238000006555 catalytic reaction Methods 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
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- 229910021645 metal ion Inorganic materials 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
- 238000004064 recycling 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
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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Abstract
The invention discloses a production method of self-bonding high-strength wood columnar activated carbon, which belongs to the technical field of production of activated carbon adsorption materials, the columnar activated carbon is produced by a phosphoric acid method, biomass and phosphoric acid are mixed and then carbonized and then granulated, the size nondeterminacy shrinkage after material granulation is reduced, the material form and size are stable, and through the thermocuring in an anoxic micro-negative pressure environment, the residual phosphate of the columnar activated carbon washing incomplete material and carbon surface functional groups are subjected to high-temperature thermocuring polycondensation modification, so that the strength and the stacking density of the columnar activated carbon are improved; the gradient recovery method of the water washing tank directly filled with the activated material in series replaces the traditional gradient recovery method of transfer transition in the gradient acid tank, so that the phosphoric acid recovery efficiency is improved, the consumption of hot water for extraction is reduced, the phosphoric acid recovery concentration is increased, and the energy conservation and consumption reduction are realized. The invention also has the advantages of simple process, high automation degree, high production efficiency and the like, and is beneficial to industrial popularization and application.
Description
Technical Field
The invention belongs to the technical field of production of activated carbon adsorption materials, and particularly relates to a production method of self-bonding high-strength wood columnar activated carbon.
Background
The common columnar activated carbon is mostly coal-based activated carbon by a physical method, and is mainly prepared by adding coal tar, asphalt and other binders into coal powder, extruding, forming, granulating and then activating by the physical method. The physical method coal-based activated carbon has high strength and large specific gravity, but has lower adsorption performance due to the limitation of physical method activation. The common phosphoric acid method wood columnar carbon is prepared by kneading, molding and granulating biomass powder after adding phosphoric acid and activating carbon, and has the defects of high adsorption performance, low strength and small specific gravity. The wood columnar activated carbon with high strength, large specific gravity and high adsorption performance in the market is less, and the production cost is higher.
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 added, metal ions are continuously enriched, the purity of phosphoric acid in a system is continuously reduced, and efficient catalysis is difficult to realize. The application number of CN201710531774.0 wood particle activated carbon for the automobile carbon tank and the preparation method thereof adopt a phosphoric acid method for primary activation and a physical method for secondary activation, the production process is complex, the cost is high, and the product ash content is high due to the adoption of an inorganic binder, so that the high-adsorption wood columnar activated carbon is difficult to obtain.
Disclosure of Invention
The invention aims to provide a method for producing self-bonding high-strength wood columnar activated carbon so as to solve the problems.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a production method of self-bonding 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) Blending and kneading: putting the biomass powder and the circulating acid obtained in the step 1) into a kneading machine with a hot water jacket for kneading to obtain a kneaded material;
3) Pre-carbonizing: conveying the kneaded material obtained in the step 2) to an internal heating type rotary furnace for dehydration and pre-carbonization to obtain a pre-carbonized material;
4) Refining into mud: conveying the pre-carbonized material obtained in the step 3) to a vacuumized extruder for extrusion molding to obtain refined columnar pug;
5) Molding a mold: conveying the refined columnar pug obtained in the step 4) to an extruder with a columnar die for granulation, and then automatically cutting to obtain granular columnar wet materials;
6) Drying and forming: drying the granular cylindrical wet material obtained in the step 5) to obtain a cylindrical dry material;
7) And (3) activation: conveying the columnar dry material obtained in the step 6) to an anoxic micro negative pressure internal heating type rotary furnace at 400-500 ℃ through a sealing feeder for activation for 1-4 h, and then cooling and discharging to obtain a columnar activated material;
8) Recovering and washing: conveying the columnar activated material obtained in the step 7) to a water washing tank for gradient recovery of phosphoric acid and washing with hot water in sequence to obtain an incomplete material of columnar activated carbon washing;
9) And (3) water filtration and drying: discharging the incompletely-washed columnar activated carbon material obtained in the step 8) from the bottom of a water washing tank, and filtering, absorbing water and drying through a mesh belt to obtain a semi-finished columnar activated carbon product;
10 Thermal curing: and (3) putting the columnar activated carbon semi-finished product obtained in the step 9) into an anoxic micro-negative pressure external heating type rotary furnace at 500-800 ℃ for thermosetting for 0.5-3 h, obtaining hot air from thermosetting flue gas through a heat exchanger for heating and drying, and then discharging and indirectly cooling to obtain the high-strength wood columnar activated carbon.
Further, the biomass powder in the step 1) is selected from any one or more of wood chip powder, bamboo chip powder, cotton seed powder and fruit shell powder; the particle size is 200 meshes, the passing rate is 95 percent, and the water content is less than 10 percent.
Further, the mass ratio of the biomass powder to the circulating acid in the step 2) is 1:2-3; the temperature of the hot water jacket is 80-100 ℃; the kneading time is 20-40 min; the circulating acid is 55-65% of phosphoric acid.
Further, the heat source of the internal heating type rotary furnace in the step 3) is hot air provided by natural gas combustion, the temperature is kept, and a thick carbon dioxide and nitrogen protective atmosphere is formed; the temperature of the internal heating type rotary furnace is 120-160 ℃, and the time for pre-carbonizing the material is 0.5-2h.
Further, the extruder in the step 4) selects a spiral pugmill, and the spiral pugmill extrudes columnar refined pug with the diameter of 10-40 mm; the pressure value of the vacuum pumping is-0.06 to-0.09 MPa.
Further, the extruder provided with the columnar die in the step 5) selects a spiral extrusion granulator with the diameter of 2-8mm, and a discharge port of the granulator is provided with a rotary cutter disc for automatic cutting.
Further, in the step 6), a multilayer mesh belt dryer is adopted to gradually dry at a temperature of 80-180 ℃ in sequence, and the moisture content is within 5% after drying; and the drying tail gas adopts a spray tower to recover waste heat to obtain a large amount of hot water, and the hot water is reused for production.
Preferably, the step 8) recovery washing is specifically as follows: adopting a water washing tank with a height-diameter ratio of more than 3 and a filter screen layer, connecting more than 6 water washing tanks filled with activated materials in series for gradient phosphoric acid recovery and gradient washing, wherein the advancing route of the activated materials is opposite to that of hot water, feeding hot water into the tank 1, discharging the gradient phosphoric acid from the tank at the tail part of the series, and purifying the obtained gradient phosphoric acid by using ion exchange resin and then recycling the purified gradient phosphoric acid for blending and kneading in the step 2); step 9) draining and drying specifically comprise: and discharging from the bottom of the water washing tank by adopting pump circulation flushing, conveying the material to a dryer through a filter screen conveying belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product.
Further, the pH value of the incompletely washed material of the columnar activated carbon in the step 8) is 1.8-3.
Furthermore, the micro negative pressure in the step 3), the step 7) and the step 10) is-5 to-200 pa.
The invention has the following advantages:
1) The method adopts a phosphoric acid method to produce the wood columnar activated carbon, mixes the ingredients, pre-carbonizes the ingredients and then granulates the ingredients, the pre-carbonization ensures that the material has stable shape and size and high-strength self-binding property, the granulated product is uniform, and the pre-carbonization has a certain dehydration function, thereby enhancing the activation and pore-forming functions and improving the productivity.
2) The invention adopts the heat curing in an anoxic micro-negative pressure environment, and the residual phosphate of the incompletely washed columnar activated carbon material and the functional groups on the surface of the carbon are subjected to heat curing polycondensation modification at high temperature, so that the strength and the bulk density of the columnar activated carbon are improved.
3) The invention adopts the tanks which are connected in series and filled with the activated material to carry out gradient recovery of heat energy and purification and concentration of phosphoric acid, the advancing route of the activated material is opposite to the advancing route of hot water, hot water is fed into the tank 1, and gradient phosphoric acid is discharged from the tank at the tail part of the string, thereby replacing the traditional phosphoric acid recovery and washing modes of a gradient phosphoric acid tank and gradient water, maintaining the high-efficiency comprehensive utilization of heat energy and reducing the unit energy consumption and acid consumption.
4) The invention has simple production process, high automation degree and high production efficiency, and is beneficial to industrial popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached figure 1, the invention provides a production method of self-bonding 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 90 percent and the moisture of 10 percent of 200 meshes; wherein the biomass powder is selected from one or more of sawdust powder, bamboo dust powder, cottonseed powder and fruit shell powder.
2) Blending and kneading: and (2) putting 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 the mass ratio of 1:2-3 for kneading for 20-40 min to obtain a kneaded material.
3) Pre-carbonizing: conveying the kneaded material obtained in the step 2) to 120-160 ℃ through a conveyer belt, dehydrating and pre-carbonizing the kneaded material for 0.5-2h by using a micro negative pressure internal heating type rotary furnace at minus 5-200 pa; the heat source of the internal heating type rotary furnace is hot air provided by natural gas combustion, the temperature is kept, and a thick carbon dioxide and nitrogen protective atmosphere is formed.
4) Refining into mud: conveying the pre-carbonized material obtained in the step 3) to a vacuumized spiral pug mill with the pressure of-0.06 to-0.09 MPa through a conveyer belt to extrude the pre-carbonized material into columnar refined pug with the diameter of 10-40mm, and obtaining the refined columnar pug;
5) Molding a mold: conveying the refined columnar pug obtained in the step 4) to an extruder with a columnar die through a conveying belt to carry out extrusion forming 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 disc to carry out automatic cutting to obtain granular columnar wet material;
6) Drying and forming: conveying the granular cylindrical wet material obtained in the step 5) to a multilayer mesh belt dryer through a conveying belt, and then gradually drying the granular cylindrical wet material at a temperature of 80-180 ℃ in sequence, wherein the moisture content is within 5% after drying to obtain a cylindrical dry material; and the drying tail gas adopts a spray tower to recover waste heat to obtain a large amount of hot water, and the hot water is reused for production.
7) And (3) activation: conveying the columnar dry material obtained in the step 6) to an anoxic micro negative pressure internal heating type rotary furnace at 400-500 ℃ and-5-200 pa through a sealed feeder, activating for 1-4 h, cooling and discharging to obtain a columnar activated material;
8) Recovering and washing: conveying the columnar activated material obtained in the step 7) to a water washing tank for gradient recovery of phosphoric acid and washing with hot water in sequence to obtain an incomplete material of columnar activated carbon washing; specifically, a water washing tank with a height-diameter ratio of more than 3 and a filter screen layer is adopted, more than 6 water washing tanks filled with activated materials are connected in series for gradient phosphoric acid recovery and gradient washing, the advancing route of the activated materials is opposite to that of hot water, hot water is fed into a tank 1, gradient phosphoric acid is discharged from a tank at the tail of the tank, and the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for ingredient kneading in the step 2); the pH value of the incompletely washed material of the columnar activated carbon is 1.8-3.
9) And (3) draining and drying: discharging the incompletely washed columnar activated carbon material from the bottom of the water washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveying belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; wherein, the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan and absorbs water on the surface of the material.
10 Thermal curing: putting the columnar activated carbon semi-finished product obtained in the step 9) into an anoxic micro-negative pressure external heating type rotary furnace at 500-800 ℃, 5-200 pa for thermosetting for 0.5-3 h, wherein the strength is enhanced by thermosetting, and meanwhile, the surface functional groups are adjusted to improve the chemical adsorption performance and reduce the product impurities. Hot air obtained by the hot curing flue gas passes through a heat exchanger and is used for heating and drying, and then the hot curing flue gas is discharged and indirectly cooled to obtain high-strength wood columnar activated carbon.
Example 1
Drying, crushing, desanding and deironing sawdust, bamboo sawdust, fruit shells and cotton seeds to obtain biomass powder with a passing rate of 90% and water content of 10% of 200 meshes, putting 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 for kneading for 20min, conveying the kneaded material to 120 ℃, dehydrating and pre-carbonizing in a micro-negative pressure internal heating type rotary furnace at minus 5-minus 200pa for 2h, and using hot air provided by natural gas combustion as an internal heating type heat source to keep the temperature and form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a screw pug mill with vacuum pumping of-0.06-0.09 MPa to extrude the pre-carbonized material into columnar refined pug with the diameter of 10-40mm, granulating the refined columnar pug in a screw extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge hole of the granulator by a rotary cutter to obtain granular columnar wet material; conveying the granular columnar wet material to a multilayer mesh belt drying machine, gradually drying at a temperature range of 80-180 ℃ in sequence, and controlling the moisture content within 5% after drying to obtain a columnar dry material; wherein, the drying tail gas adopts a spray tower to recover waste heat to obtain a large amount of hot water which is reused for production.
Conveying the columnar dry material to an anoxic micro negative pressure internal heating type rotary furnace at 400 ℃ and minus 5 to minus 200pa through a sealed feeder, activating for 4 hours, cooling and discharging to obtain a 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 for gradient recovery of phosphoric acid and gradient washing, the advancing route of the activated material is opposite to that of hot water, hot water is fed into a tank 1, gradient phosphoric acid is discharged from a tank at the tail of the tank, the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for kneading of the ingredients, and the pH of the obtained incompletely washed columnar activated carbon material is 3; discharging the incompletely washed columnar activated carbon material from the bottom of the water washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveyor belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan, water on the surface of the material is absorbed, the columnar activated carbon semi-finished product is put into an anoxic micro-negative pressure external heating type rotary furnace at 800 ℃, 5 to 200pa for thermal curing for 3 hours, hot air obtained by the thermal curing flue gas through a heat exchanger is used for heating and drying, and then the material is discharged for indirect cooling to obtain the high-strength wood columnar activated carbon.
Example 2
Drying, crushing, desanding and deironing sawdust, bamboo sawdust, fruit shells and cotton seeds to obtain biomass powder with a passing rate of 90% and water content of 10% of 200 meshes, putting 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 for kneading for 20min, conveying the kneaded material to 120 ℃, dehydrating and pre-carbonizing in a micro-negative pressure internal heating type rotary furnace at minus 5-minus 200pa for 2h, and using hot air provided by natural gas combustion as an internal heating type heat source to keep the temperature and form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a screw pug mill with vacuum pumping of-0.06-0.09 MPa to extrude the pre-carbonized material into columnar refined pug with the diameter of 10-40mm, granulating the refined columnar pug in a screw extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge hole of the granulator by a rotary cutter to obtain granular columnar wet material; conveying the granular columnar wet material to a multilayer mesh belt drying machine, gradually drying at a temperature range of 80-180 ℃ in sequence, and controlling the moisture content within 5% after drying to obtain a columnar dry material; wherein, the drying tail gas adopts a spray tower to recover waste heat to obtain a large amount of hot water which is reused for production.
Conveying the columnar dry material to an anoxic micro negative pressure internal heating type rotary furnace at 400 ℃ and minus 5 to minus 200pa through a sealed feeder, activating for 4 hours, cooling and discharging to obtain a 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 for gradient recovery of phosphoric acid and gradient washing, the advancing route of the activated material is opposite to that of hot water, hot water is fed into the tank 1, gradient phosphoric acid is discharged from the tank at the tail of the tank, the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for kneading of the ingredients, and the pH of the obtained columnar activated carbon washing incomplete material is 1.8; discharging the incompletely washed columnar activated carbon material from the bottom of the water washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveyor belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan, water on the surface of the material is absorbed, the columnar activated carbon semi-finished product is put into an anoxic micro-negative pressure external heating type rotary furnace at 500 ℃, 5 to-200 pa for thermal curing for 3 hours, hot air obtained by the thermal curing flue gas through a heat exchanger is used for heating and drying, and then the material is discharged and indirectly cooled to obtain the high-strength wooden columnar activated carbon.
Example 3
Drying, crushing, desanding and deironing sawdust, bamboo chips and fruit shells to obtain biomass powder with a passing rate of 90% and water content of 10% of 200 meshes, putting the biomass powder and 60% of circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to the mass ratio of 1:3 for kneading for 30min, conveying the kneaded material to 130 ℃, dehydrating and pre-carbonizing in a micro-negative pressure internal heating type rotary furnace at minus 5-minus 200pa for 1.5h, and using hot air provided by natural gas combustion as an internal heating source to keep the temperature and form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a screw pug mill with vacuum pumping of-0.06-0.09 MPa to extrude the pre-carbonized material into columnar refined pug with the diameter of 10-40mm, granulating the refined columnar pug in a screw extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge hole of the granulator by a rotary cutter to obtain granular columnar wet material; conveying the granular columnar wet material to a multilayer mesh belt drying machine, gradually drying at a temperature of 80-180 ℃, and controlling the moisture content within 5% after drying to obtain a columnar dry material; wherein, the drying tail gas adopts a spray tower to recover the waste heat to obtain a large amount of hot water for reuse in production.
Conveying the columnar dry material to an anoxic micro-negative pressure internal heating type rotary furnace at 450 ℃ -minus 5-minus 200pa through a sealed feeder, activating for 2 hours, and then cooling and discharging to obtain a 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 for gradient recovery of phosphoric acid and gradient washing, the advancing route of the activated material is opposite to that of hot water, hot water is fed into a tank 1, gradient phosphoric acid is discharged from a tank at the tail of the tank, the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for kneading of the ingredients, and the pH of the obtained incompletely washed columnar activated carbon material is 3; discharging the incompletely washed columnar activated carbon material from the bottom of the water washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveyor belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan, water on the surface of the material is absorbed, the columnar activated carbon semi-finished product is put into an anoxic micro negative pressure external heating type rotary furnace at 600 ℃, 5 to 200pa for thermal curing for 2 hours, hot air obtained by the thermal curing flue gas through a heat exchanger is used for heating and drying, and then the material is discharged for indirect cooling to obtain the high-strength wood columnar activated carbon.
Example 4
Drying, crushing, desanding and deironing wood chips, bamboo chips, shells and cotton seeds to obtain biomass powder with a 200-mesh passing rate of 90% and water content of 10%, adding the biomass powder and 65% of 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 145 ℃, dehydrating and pre-carbonizing for 1h in a micro-negative pressure internal heating type rotary furnace at-5 to-200 pa, wherein an internal heating type heat 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 screw pug mill with vacuum pumping of-0.06-0.09 MPa to extrude the pre-carbonized material into columnar refined pug with the diameter of 10-40mm, granulating the refined columnar pug in a screw extrusion granulator with the granulation diameter of 2-8mm, and automatically cutting a discharge hole of the granulator by a rotary cutter to obtain granular columnar wet material; conveying the granular columnar wet material to a multilayer mesh belt drying machine, gradually drying at a temperature range of 80-180 ℃ in sequence, and controlling the moisture content within 5% after drying to obtain a columnar dry material; wherein, the drying tail gas adopts a spray tower to recover the waste heat to obtain a large amount of hot water for reuse in production.
Conveying the columnar dry material to an anoxic micro-negative pressure internal heating type rotary furnace at 480 ℃ and minus 5 to minus 200pa through a sealed feeder, activating for 1 hour, and then cooling and discharging to obtain a 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 for gradient recovery of phosphoric acid and gradient washing, the advancing route of the activated material is opposite to that of hot water, hot water is fed into a tank 1, gradient phosphoric acid is discharged from a tank at the tail of the tank, the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for kneading of the ingredients, and the pH of the obtained columnar activated carbon washing incomplete material is 2.8; discharging the incompletely-washed columnar activated carbon material from the bottom of the washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveyor belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan, water on the surface of the material is absorbed, the columnar activated carbon semi-finished product is put into an anoxic micro-negative pressure external heating type rotary furnace at 700 ℃, minus 5 to minus 200pa for thermal curing for 1 hour, hot air obtained by the thermal curing flue gas through a heat exchanger is used for heating and drying, and then the material is discharged and indirectly cooled to obtain the high-strength wooden columnar activated carbon.
Example 5
Drying, crushing, desanding and deironing sawdust, bamboo chips and fruit shells to obtain biomass powder with a passing rate of 90% and water content of 10% of 200 meshes, putting the biomass powder and 55% of circulating phosphoric acid into a kneader with a hot water jacket at 80-100 ℃ according to the mass ratio of 1:3 for kneading for 30min, conveying the kneaded material to 160 ℃, dehydrating and pre-carbonizing for 0.5h by a micro-negative pressure internal heating type rotary furnace at minus 5-minus 200pa, and keeping the temperature by using hot air provided by natural gas combustion to form a thick carbon dioxide and nitrogen protective atmosphere; conveying the pre-carbonized material to a screw pugmill with vacuum pumping of-0.06-0.09 MPa to extrude the pre-carbonized material into columnar refined pugmill with the diameter of 10-40mm, granulating the refined columnar pugmill by a screw 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 material; conveying the granular columnar wet material to a multilayer mesh belt drying machine, gradually drying at a temperature range of 80-180 ℃ in sequence, and controlling the moisture content within 5% after drying to obtain a columnar dry material; wherein, the drying tail gas adopts a spray tower to recover waste heat to obtain a large amount of hot water which is reused for production.
Conveying the columnar dry material to an anoxic micro negative pressure internal heating type rotary furnace at 500 ℃ and minus 5 to minus 200pa through a sealed feeder, activating for 4 hours, cooling and discharging to obtain a 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 for gradient recovery of phosphoric acid and gradient washing, the advancing route of the activated material is opposite to that of hot water, hot water is fed into a tank 1, gradient phosphoric acid is discharged from a tank at the tail of the tank, the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for kneading of the ingredients, and the pH of the obtained columnar activated carbon washing incomplete material is 2.5; discharging the incompletely washed columnar activated carbon material from the bottom of the water washing tank by adopting pump circulating flushing, conveying the material to a dryer by a filter screen conveyor belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product; the water absorption device consists of a water absorption disc, a cyclone separator and a high-pressure fan, water on the surface of the material is absorbed, the columnar activated carbon semi-finished product is put into an anoxic micro negative pressure external heating type rotary furnace at 800 ℃, 5 to 200pa for thermal curing for 0.5h, hot air obtained by the hot curing flue gas through a heat exchanger is used for heating and drying, and then the material is discharged for indirect cooling to obtain the high-strength wood columnar activated carbon.
Comparative example 1
The technical scheme of the comparative example is basically the same as that of example 1, except that the pH of the incompletely washed columnar activated carbon material after washing is 1.5.
Comparative example 2
The technical scheme of the comparative example is basically the same as that of example 1, except that the pH of the incompletely washed columnar activated carbon material after washing is 1.0.
Comparative example 3
The technical scheme of the comparative example is basically the same as that of example 1, except that the pH of the incompletely washed columnar activated carbon material after washing is 3.5.
Comparative example 4
The technical scheme of the comparative example is basically the same as that of example 1, except that the pH of the incompletely washed columnar activated carbon material after washing is 4.0.
Comparative example 5
The technical solution of the comparative example is substantially the same as that of example 5, except that the thermosetting temperature of the columnar activated carbon semi-finished product is 900 ℃.
Comparative example 6
The technical solution of the comparative example is substantially the same as that of example 5, except that the thermosetting temperature of the columnar activated carbon semi-finished product is 850 ℃.
Comparative example 7
The technical solution of the comparative example is substantially the same as that of example 5, except that the thermosetting temperature of the columnar activated carbon semi-finished product is 450 ℃.
Comparative example 8
The technical solution of the comparative example is substantially the same as that of example 5, except that the thermosetting temperature of the columnar activated carbon semi-finished product is 400 ℃.
Product performance detection
The indexes of the activated carbon prepared in examples 1 to 5 and comparative examples 1 to 8, such as adsorption performance, particle size and the like, were measured, and the results are shown in the following table:
strength test reference: GB/T12496.6-1999 strength determination of wood active carbon test method
It can be seen from the above data that the adsorption performance and strength of the columnar activated carbon prepared in examples 1 to 5 of the present invention are superior to those of the commercially available columnar activated carbon, i.e., the columnar activated carbon prepared in the present invention has not only higher strength but also superior adsorption performance.
Comparing the data of examples 1-2 and comparative examples 1-4, it can be seen that when the pH of the incompletely washed material of columnar activated carbon is too low, the adsorption value is lowered and the ash content is increased. 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 material of the columnar activated carbon is too high. Therefore, experimental data show that when the pH value of the incompletely washed material of the columnar activated carbon is 1.8-3, the prepared activated carbon has good strength and adsorption performance, and the ash content is low.
As can be seen from the data of comparative example 5 and comparative examples 5 to 8, the adsorption performance of the activated carbon generally decreases as the heat curing temperature of the columnar activated carbon semi-finished product increases. When the temperature is less than 500 ℃, the strength of the activated carbon tends to decrease and ash content increases. The invention comprehensively considers the energy consumption, the strength of the active carbon and the adsorption performance, so the heat curing temperature is 500-800 ℃.
The above-mentioned embodiments, which further illustrate the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned embodiments are only preferred embodiments of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A production method of self-bonding high-strength wood columnar activated carbon is characterized by comprising the following steps:
1) Pretreatment of raw materials: drying, crushing, desanding and deironing the three residues of the biomass to obtain biomass powder;
2) Blending and kneading: putting the biomass powder obtained in the step 1) and circulating acid into a kneading machine with a hot water jacket for kneading to obtain a kneaded material;
3) Pre-carbonization: conveying the kneaded material obtained in the step 2) to a micro-negative pressure internal heating type rotary furnace for dehydration and pre-carbonization to obtain a pre-carbonized material;
4) Refining into mud: conveying the pre-carbonized material obtained in the step 3) to a vacuumized extruder for extrusion molding to obtain refined columnar pug;
5) Molding a mold: conveying the refined columnar pug obtained in the step 4) to an extruder with a columnar die for granulation, and then automatically cutting to obtain granular columnar wet materials;
6) Drying and forming: drying the granular cylindrical wet material obtained in the step 5) to obtain a cylindrical dry material;
7) And (3) activation: conveying the columnar dry material obtained in the step 6) to an anoxic micro negative pressure internal heating type rotary furnace at 400-500 ℃ through a sealing feeder for activation for 1-4 h, and then cooling and discharging to obtain a columnar activated material;
8) Serial recovery washing: conveying the columnar activated material obtained in the step 7) to a water washing tank connected in series for gradient recovery of phosphoric acid and washing with hot water in sequence, wherein the traveling route of the activated material is opposite to that of the hot water, hot water is fed into a tank 1 in series, and gradient phosphoric acid is discharged from a tank at the tail of the series to obtain an incomplete material for washing with columnar activated carbon;
9) And (3) draining and drying: discharging the incompletely-washed columnar activated carbon material obtained in the step 8) from the bottom of a water washing tank, and filtering, absorbing water and drying through a mesh belt to obtain a semi-finished columnar activated carbon product;
10 Thermal curing: and (3) putting the columnar activated carbon semi-finished product obtained in the step 9) into an anoxic micro-negative pressure external heating type rotary furnace at 500-800 ℃ for thermosetting for 0.5-3 h, obtaining hot air from thermosetting flue gas through a heat exchanger for heating and drying, and then discharging and indirectly cooling to obtain the high-strength wood columnar activated carbon.
2. The method for producing a self-bonded high-strength wooden columnar activated carbon as claimed in claim 1, wherein the biomass powder in step 1) is any one or more of wood dust powder, bamboo dust powder, cotton seed powder and fruit shell powder; the particle size is more than 95% of 200 meshes of passing rate and less than 10% of water.
3. The method for producing self-bonding high-strength woody columnar activated carbon as claimed in claim 1, wherein the mass ratio of the biomass powder to the circulating acid in the step 2) is 1:2-3; the temperature of the hot water jacket is 80-100 ℃; the kneading time is 20-40 min; the circulating acid is 55-65% of phosphoric acid.
4. The method for producing a self-bonding high-strength wooden columnar activated carbon as claimed in claim 1, wherein the heat source of the internal heating type rotary kiln in the step 3) is hot air supplied by burning natural gas, the temperature is maintained, and a protective atmosphere of dense carbon dioxide and nitrogen is formed; the temperature of the internal heating type rotary furnace is 120-160 ℃, and the time for pre-carbonizing the material is 0.5-2h.
5. The method for producing a self-binding high-strength wooden columnar activated carbon as claimed in claim 1, wherein the extruder in step 4) is a screw pugmill extruding columnar refined pugs with a diameter of 10-40 mm; the pressure value of the vacuum pumping is-0.06 to-0.09 MPa.
6. The method for producing a self-bonded high-strength wooden columnar activated carbon as claimed in claim 1, wherein the extruder equipped with the columnar die in step 5) is a screw extrusion granulator with a diameter of 2-8mm, and a discharge port of the granulator is equipped with a rotary cutter head for automatic cutting.
7. The method for producing a self-bonding high-strength wooden columnar activated carbon as claimed in claim 1, wherein a multi-layer mesh belt dryer is adopted in step 6) to gradually dry at a temperature of 80-180 ℃ in sequence, and the moisture content after drying is within 5%.
8. The process for producing a self-bonded high-strength woody columnar activated carbon as claimed in claim 1, wherein the recovering and washing of the step 8) is specifically: adopting a water washing tank with a height-diameter ratio of more than 3 and a filter screen layer, connecting more than 6 water washing tanks filled with activated materials in series for gradient phosphoric acid recovery and gradient washing, wherein the advancing route of the activated materials is opposite to the advancing route of hot water, the water is fed into the tank 1, the gradient phosphoric acid is discharged from the tank at the tail part of the series, and the obtained gradient phosphoric acid is purified by ion exchange resin and then is recycled for blending and kneading in the step 2); step 9), draining and drying specifically comprise: and discharging from the bottom of the water washing tank by adopting pump circulation flushing, conveying the material to a dryer through a filter screen conveying belt with a water absorption device, and drying until the water content is within 5% to obtain a columnar activated carbon semi-finished product.
9. A process for producing a self-binding high strength woody columnar activated carbon as claimed in claim 1, wherein the pH of the incompletely washed material of the columnar activated carbon in the step 8) is 1.8 to 3.
10. The method for producing a self-bonded high-strength woody columnar activated carbon as claimed in claim 1, wherein the micro-negative pressures in the steps 3), 7) and 10) are all from-5 to-200 pa.
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