CN109336108B - Water purification activated carbon and preparation method thereof - Google Patents
Water purification activated carbon and preparation method thereof Download PDFInfo
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- CN109336108B CN109336108B CN201811454582.5A CN201811454582A CN109336108B CN 109336108 B CN109336108 B CN 109336108B CN 201811454582 A CN201811454582 A CN 201811454582A CN 109336108 B CN109336108 B CN 109336108B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 119
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000000746 purification Methods 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims description 36
- 239000000843 powder Substances 0.000 claims abstract description 59
- 244000276331 Citrus maxima Species 0.000 claims abstract description 47
- 235000001759 Citrus maxima Nutrition 0.000 claims abstract description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 230000003213 activating effect Effects 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 239000005539 carbonized material Substances 0.000 claims description 34
- 239000002253 acid Substances 0.000 claims description 32
- 238000002791 soaking Methods 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 21
- 239000004744 fabric Substances 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 14
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 13
- 239000000845 maltitol Substances 0.000 claims description 13
- 235000010449 maltitol Nutrition 0.000 claims description 13
- 229940035436 maltitol Drugs 0.000 claims description 13
- 238000007873 sieving Methods 0.000 claims description 13
- 229960002920 sorbitol Drugs 0.000 claims description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000010298 pulverizing process Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 11
- 150000005846 sugar alcohols Polymers 0.000 claims description 11
- 239000012190 activator Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- ZJDOESGVOWAULF-OGJQONSISA-N Geniposidic acid Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@@H]2C(CO)=CC[C@@H]2C(C(O)=O)=CO1 ZJDOESGVOWAULF-OGJQONSISA-N 0.000 claims description 9
- VYAALAFRWREWLA-BVTMAQQCSA-N Geniposidic acid Natural products CCC1=CC[C@H]2[C@@H]1[C@H](O[C@@H]3O[C@H](CO)[C@@H](O)[C@H](O)[C@H]3O)OC=C2C(=O)O VYAALAFRWREWLA-BVTMAQQCSA-N 0.000 claims description 8
- ZJDOESGVOWAULF-UHFFFAOYSA-N Geniposidinsaeure Natural products OC1C(O)C(O)C(CO)OC1OC1C2C(CO)=CCC2C(C(O)=O)=CO1 ZJDOESGVOWAULF-UHFFFAOYSA-N 0.000 claims description 8
- BZPMXJKRKXDRID-UOIKKKDVSA-N Scandoside Natural products OC[C@H]1O[C@@H](O[C@H]2CC=C([C@@H]3[C@@H](O)C=C(CO)[C@H]23)C(=O)O)[C@H](O)[C@@H](O)[C@@H]1O BZPMXJKRKXDRID-UOIKKKDVSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229920005862 polyol Polymers 0.000 claims description 8
- 150000003077 polyols Chemical class 0.000 claims description 8
- 229940074391 gallic acid Drugs 0.000 claims description 5
- 235000004515 gallic acid Nutrition 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000008213 purified water Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 18
- 238000005470 impregnation Methods 0.000 abstract description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052740 iodine Inorganic materials 0.000 abstract description 7
- 239000011630 iodine Substances 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 238000010000 carbonizing Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000001963 growth medium Substances 0.000 description 6
- 239000010902 straw Substances 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 4
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000811 xylitol Substances 0.000 description 3
- 235000010447 xylitol Nutrition 0.000 description 3
- 229960002675 xylitol Drugs 0.000 description 3
- IBFYXTRXDNAPMM-BVTMAQQCSA-N Geniposide Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1C(=CC2)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O IBFYXTRXDNAPMM-BVTMAQQCSA-N 0.000 description 2
- IBFYXTRXDNAPMM-FZEIBHLUSA-N Geniposide Natural products COC(=O)C1=CO[C@@H](O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O)[C@H]2[C@@H]1CC=C2CO IBFYXTRXDNAPMM-FZEIBHLUSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- VGLLGNISLBPZNL-RBUKDIBWSA-N arborescoside Natural products O=C(OC)C=1[C@@H]2C([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)=C(CO)CC2 VGLLGNISLBPZNL-RBUKDIBWSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 ester compound Chemical class 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000620209 Escherichia coli DH5[alpha] Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- LPSCRKGVODJZIB-UHFFFAOYSA-N [I].[C] Chemical class [I].[C] LPSCRKGVODJZIB-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940041514 candida albicans extract Drugs 0.000 description 1
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 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
- 239000012137 tryptone Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000012138 yeast extract Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
Abstract
The invention discloses high-efficiency water purification activated carbon. The high-efficiency water purification activated carbon is obtained by immersing coarse shaddock peel powder in an activating agent at normal pressure and high pressure, carbonizing under the protection of nitrogen, and acidifying. Compared with the prior art, the high-efficiency water purification activated carbon disclosed by the invention has the advantages that the activating agent is promoted to permeate into the internal structure of the shaddock peel coarse powder through high-pressure impregnation, the impregnation effect is improved, and a series of crosslinking, dehydration and polycondensation reactions are carried out at high temperature in the later stage to prepare the activated carbon with large specific surface area and more surface functional groups. The high-efficiency water purification activated carbon not only has high iodine adsorption value, specific surface area and pore volume, can effectively filter impurities in water, but also has remarkable antibacterial effect, can be used as a filter element of water purification equipment for a long time, and has low cost, large adsorption capacity, good adsorption performance and no secondary pollution.
Description
Technical Field
The invention relates to the technical field of activated carbon, in particular to high-efficiency water purification activated carbon and a preparation method thereof.
Background
Along with the acceleration of the urbanization process, the increase of urban population and the enhancement of environmental awareness, the discharge amount of urban industrial wastewater and domestic sewage is increasing day by day, the urban sewage treatment rate is also improved year by year, and the sludge production rate of sewage plants is also increased sharply. The water treatment agent mainly comprises agents required by technologies such as corrosion inhibitors, scale inhibition and dispersion agents, sterilization and algae removal agents, flocculating agents, ion exchange resins, purifying agents, cleaning agents, prefilming agents and the like, for treating cooling water and boiler water, desalting seawater, separating membranes, biologically treating, flocculating, exchanging ions and the like.
The activated carbon has a large specific surface area and a developed void structure, so that the activated carbon has strong adsorption capacity on dissolved organic matters such as phenolic compounds and the like in water and is suitable for purifying drinking water. The active carbon products adopted in the current market are mainly of two types, namely, the active carbon products are prepared from columnar active carbon or raw coal is directly crushed, and the two types of products have the defect which is difficult to solve when used for purifying water quality and are difficult to achieve the purpose of purifying the water quality.
In the prior art, Chinese patent CN201710466241.9 proposes a high-efficiency water purification activated carbon, which is prepared by the following steps: drying the straws, crushing and sieving the straws to 10-60 meshes, and uniformly mixing the straws; carrying out primary carbonization in a microwave cracking reaction furnace to prepare a pretreatment material; the microwave power is 1000-; soaking the pretreated material in 15-35 wt% hydrochloric acid solution for 3-20h, then soaking in 15-30 wt% sodium hydroxide solution for-5 h, repeatedly washing with deionized water until neutral, and drying to obtain a semi-finished product; and (4) placing the semi-finished product into a muffle furnace with the temperature of 380-420 ℃ for heat preservation treatment for 0.5-2h, and cooling to room temperature to obtain the product. The invention reduces the production cost to a certain extent by using the straws, but mesopores and macropores with better adsorption capacity are formed on the surface of the straws in the carbonization process, so that the adsorption capacity of the straws is reduced, and the aim of purifying water quality is difficult to achieve.
The invention provides high-efficiency water purification activated carbon which is obtained by impregnating coarse shaddock peel powder in an activating agent at normal pressure, impregnating the coarse shaddock peel powder at high pressure, carbonizing the coarse shaddock peel powder under the protection of nitrogen and acidifying the carbonized shaddock peel powder. Compared with the prior art, the high-efficiency water purification activated carbon has a good water purification effect.
Disclosure of Invention
The invention aims to provide high-efficiency water purification activated carbon. The shaddock peel coarse powder is soaked in an activating agent at normal pressure and high pressure, carbonized under the protection of nitrogen and acidified to obtain the shaddock peel coarse powder; has high iodine adsorption value, specific surface area and pore volume, can effectively filter impurities in water, and has good water purification performance.
The specific technical scheme is as follows:
a preparation method of high-efficiency water purification activated carbon comprises the following steps:
(1) cleaning pericarpium Citri Grandis, drying, pulverizing, and sieving to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the coarse shaddock peel powder and an activating agent, and performing normal-pressure impregnation, high-pressure impregnation and filtration to obtain a filter cake, namely the impregnated coarse shaddock peel powder;
(3) carbonizing the soaked shaddock peel coarse powder at high temperature under the protection of nitrogen to obtain a carbonized material;
(4) and (3) uniformly mixing the carbonized material and the acid liquor, and carrying out normal-pressure impregnation, filtration, washing and drying to obtain the high-efficiency water purification activated carbon.
In another technical scheme, the preparation method of the high-efficiency water purification activated carbon comprises the following steps:
(1) cleaning pericarpium Citri Grandis, drying, pulverizing, and sieving to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the coarse shaddock peel powder and an activating agent, and performing normal-pressure impregnation, high-pressure impregnation and filtration to obtain a filter cake, namely the impregnated coarse shaddock peel powder;
(3) carbonizing the soaked shaddock peel coarse powder at high temperature under the protection of nitrogen to obtain a carbonized material;
(4) and (3) uniformly mixing the carbonized material and the acid liquor, and carrying out normal-pressure impregnation, filtration, washing and drying to obtain the high-efficiency water purification activated carbon.
Preferably, the preparation method of the high-efficiency water purification activated carbon comprises the following steps:
(1) cleaning pericarpium Citri Grandis, drying at 100-110 deg.C for 4-8 hr, pulverizing, and sieving with 20-50 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-to-liquid ratio of 1g (3-6) m L, soaking for 90-180 minutes under normal pressure, then soaking for 20-30 minutes under 70-90MPa, and filtering by using 200-mesh filter cloth with 500 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 600 ℃ at the speed of 8-12 ℃/min under the protection of nitrogen, and preserving the heat at 600 ℃ of 300 ℃ for 60-90 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to a solid-to-liquid ratio of 1g (3-6) m L, soaking for 20-40 minutes at normal pressure, filtering by using 200-mesh and 500-mesh filter cloth, washing the obtained solid with deionized water until the pH value of the washing liquor is 7, and drying at 80-90 ℃ until the weight is constant to obtain the high-efficiency water purification activated carbon;
the preparation method of the activating agent comprises the following steps: sequentially adding 5-10 parts by weight of phosphoric acid and 3-6 parts by weight of polyol into 30-40 parts by weight of water, and stirring for 10-20 minutes to obtain an activating agent;
the polyalcohol is one or more of D-sorbitol, maltitol and xylitol; further preferably, the polyol is preferably a mixture of D-sorbitol and maltitol, wherein the mass ratio of D-sorbitol to maltitol is (1-5): 1.
The preparation method of the acid liquor comprises the following steps: adding 0.1-0.5 part by weight of geniposidic acid and 0.5-1.0 part by weight of gallic acid into 10-15 parts by weight of water, stirring for 5-10 minutes to obtain a mixed solution, adding 10-15 parts by weight of 25-35 wt% hydrochloric acid into the mixed solution, and stirring for 10-20 minutes to obtain the acid solution.
The efficient water purification activated carbon is prepared by the preparation method of the efficient water purification activated carbon.
The invention has the beneficial effects that:
the high-efficiency water purification activated carbon has high iodine adsorption value, specific surface area and pore volume, can effectively filter impurities in water, and has good water purification performance. Moreover, the high-efficiency water purification activated carbon also has a remarkable antibacterial effect, can be used as a filter element of water purification equipment for a long time, and has the advantages of low cost, large adsorption capacity, good adsorption performance and no secondary pollution.
Detailed Description
And (3) iodine adsorption value determination: GB/T12496.8-2015 test method for Wood activated carbon iodine adsorption value determination.
Specific surface area measurement: specific surface area refers to the surface area per unit mass of solid material, i.e. the total surface area per gram of material, in m2(ii) in terms of/g. The specific surface area of the high-efficiency water-purifying activated carbon obtained in the examples was measured by using a NOVA1200 type specific surface area and porosity analyzer manufactured by Quantachrome corporation, usa. Before adsorption and sample measurement, a sample is denitrified at 120 ℃ for 3h, nitrogen is used as an adsorbate, adsorption is carried out at the liquid nitrogen temperature of 77K, and the specific surface area is calculated by using a Brunaner-Emmett-Teller (BET) equation. The total pore volume was calculated from the volume of liquid nitrogen adsorbed at a relative pressure of 0.99 according to the BarrrttJoyner and Halenda (BJH) models.
And (3) antibacterial performance test, wherein escherichia coli DH5 α and staphylococcus aureus ATCC29213 are selected as experimental strains, and a L B culture medium is adopted as a culture medium.
The experiment adopts a shaking flask method to prepare L B culture medium, 0.1g of the high-efficiency water purification activated carbon obtained in the example is respectively put into conical flasks with plugs filled with 100m L culture medium, and escherichia coli is respectively inoculated into the culture medium, so that the initial bacterial liquid concentration is 1.0 × 105cfu/m L, the cells were placed in a constant temperature shaking incubator and subjected to shaking culture at 37 ℃ and the concentration of the cells was measured by the dilution plate method at the time of 150 minutes of culture.
L B solid culture medium comprising 1% tryptone, 0.5% yeast extract powder, 1% sodium chloride, 1.5% agar powder, and distilled water.
The preparation method comprises adding distilled water into the above materials, stirring to dissolve, adjusting pH to 7.2 with 0.1 mol/L sodium hydroxide solution, and autoclaving at 121 deg.C for 30 min.
Phosphoric acid, CAS No.: 7664-38-2, available from Shanghai Michelin Biotechnology, Inc., product number: p816337, 85 wt%.
D-sorbitol, CAS No.: 50-70-4, available from Shanghai Michelin Biotechnology, Inc., product number: D817607.
maltitol, CAS number: 585-88-6, available from carbofuran technologies, inc, product number: 375445.
Xylitol, CAS No.: 87-99-0, available from Shanghai Michelin Biotechnology Ltd, product number: product numbering: x820544.
Geniposide, CAS No.: 27741-01-1, available from Shanghai-derived leaf Biotech, Inc.
Gallic acid, CAS No.: 149-91-7, Kyowa Hodgman, Inc.
The shaddock peel is obtained from fresh tribute water white shaddock provided by Yueshan mountain family farm Co.
Example 1
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 150 minutes at normal pressure, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid was added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 2
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid was added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 3
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyol is D-sorbitol.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 4
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyol is maltitol.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 5
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyol is xylitol.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 6
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyhydric alcohol is a mixture of D-sorbitol and maltitol, and the mass ratio of the D-sorbitol to the maltitol is 3: 1.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of geniposidic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
Example 7
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyhydric alcohol is a mixture of D-sorbitol and maltitol, and the mass ratio of the D-sorbitol to the maltitol is 3: 1.
The preparation method of the acid liquor comprises the following steps of: adding 1 part of gallic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
The iodine adsorption value of the obtained high-efficiency water purification activated carbon is 942.18mg/g, and the concentration of escherichia coli is 412cfu/m L.
Example 8
The preparation method of the efficient water purification activated carbon comprises the following steps of:
(1) cleaning pericarpium Citri Grandis, drying at 105 deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-liquid ratio of 1g to 4m L, soaking for 120 minutes at normal pressure, then soaking for 30 minutes at 80MPa, and filtering by using filter cloth of 200 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 450 ℃ at a speed of 10 ℃/min under the protection of nitrogen, and preserving the heat at 450 ℃ for 80 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to the solid-to-liquid ratio of 1g to 4m L, soaking for 30 minutes under normal pressure, filtering by adopting 200-mesh filter cloth, washing the obtained solid by deionized water until the pH value of the washing liquor is 7, and drying at 85 ℃ to constant weight to obtain the high-efficiency water purification activated carbon.
The preparation method of the activating agent comprises the following steps of: 8 parts of phosphoric acid and 4 parts of polyhydric alcohol were sequentially added to 35 parts of water, and stirred at 200 rpm for 15 minutes to obtain an activator.
The polyhydric alcohol is a mixture of D-sorbitol and maltitol, and the mass ratio of the D-sorbitol to the maltitol is 3: 1.
The preparation method of the acid liquor comprises the following steps of: adding 0.2 part of geniposide and 0.8 part of gallic acid into 12 parts of water, stirring for 8 minutes at 200 revolutions per minute to obtain a mixed solution, adding 12 parts of 30 wt% hydrochloric acid into the mixed solution, and stirring for 15 minutes at 200 revolutions per minute to obtain an acid solution.
The iodine adsorption value of the obtained high-efficiency water purification activated carbon is 1106.47mg/g, and the concentration of escherichia coli is 296cfu/m L.
Test example 1
The iodine adsorption value, the specific surface area and the pore volume of the high-efficiency water purification activated carbon obtained in the example are tested, and the specific results are shown in table 1.
Table 1 table of performance test results of high efficiency water purification activated carbon
Embodiment 2 adopts high-pressure impregnation to promote the activator to permeate into the internal structure of the shaddock peel coarse powder, improves the impregnation effect, and carries out a series of crosslinking, dehydration and polycondensation reactions at high temperature in the later stage to prepare the activated carbon with large specific surface area and more surface functional groups.
In example 3, a polyol was added, phosphoric acid reacted with the polyol to produce an ester compound, and the produced ester compound was easily volatilized at high temperature and decomposed to promote the formation of pores in the activated carbon. Meanwhile, substances generated by decomposition enable the activated carbon to have more surface functional groups, and the adsorption effect is improved.
Test example 2
The antibacterial properties of the high-efficiency water purification activated carbon obtained in the example were tested, and the specific results are shown in table 2.
Table 2 table of the antibacterial performance test results of the high efficiency water purification activated carbon
| E.coli concentration, cfu/m L | |
| Example 1 | 698 |
| Example 2 | 613 |
| Example 3 | 525 |
| Example 4 | 537 |
| Example 5 | 573 |
| Example 6 | 456 |
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (4)
1. The preparation method of the water purification activated carbon is characterized by comprising the following steps:
(1) cleaning pericarpium Citri Grandis, drying at 100-110 deg.C for 4-8 hr, pulverizing, and sieving with 20-50 mesh sieve to obtain pericarpium Citri Grandis coarse powder;
(2) uniformly mixing the shaddock ped coarse powder and an activating agent according to a solid-to-liquid ratio of 1g (3-6) m L, soaking for 90-180 minutes under normal pressure, then soaking for 20-30 minutes under 70-90MPa, and filtering by using 200-mesh filter cloth with 500 meshes to obtain solid, namely soaked shaddock ped coarse powder;
(3) placing the soaked shaddock ped coarse powder into a tubular furnace, heating to 600 ℃ at the speed of 8-12 ℃/min under the protection of nitrogen, and preserving the heat at 600 ℃ of 300 ℃ for 60-90 min to obtain a carbonized material;
(4) taking out the carbonized material, uniformly mixing the carbonized material with acid liquor according to a solid-to-liquid ratio of 1g (3-6) m L, soaking for 20-40 minutes at normal pressure, filtering by using 200-mesh and 500-mesh filter cloth, washing the obtained solid with deionized water until the pH value of the washing liquor is 7, and drying at 80-90 ℃ until the weight is constant to obtain purified water activated carbon;
the preparation method of the activating agent comprises the following steps: and sequentially adding 5-10 parts by weight of phosphoric acid and 3-6 parts by weight of polyol into 30-40 parts by weight of water, and stirring for 10-20 minutes to obtain the activator.
2. The method for preparing water purifying activated carbon as claimed in claim 1, wherein: the polyhydric alcohol is a mixture of D-sorbitol and maltitol, and the mass ratio of the D-sorbitol to the maltitol is (1-5): 1.
3. The method for preparing water purification activated carbon according to claim 1, wherein the method for preparing the acid solution comprises the following steps: adding 0.1-0.5 part by weight of geniposidic acid and 0.5-1.0 part by weight of gallic acid into 10-15 parts by weight of water, stirring for 5-10 minutes to obtain a mixed solution, adding 10-15 parts by weight of 25-35 wt% hydrochloric acid into the mixed solution, and stirring for 10-20 minutes to obtain the acid solution.
4. A water purifying activated carbon characterized by being prepared by the method for preparing water purifying activated carbon according to any one of claims 1 to 3.
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