CN102600800A - Preparation method of semi-coke adsorbent - Google Patents
Preparation method of semi-coke adsorbent Download PDFInfo
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- CN102600800A CN102600800A CN2012100982400A CN201210098240A CN102600800A CN 102600800 A CN102600800 A CN 102600800A CN 2012100982400 A CN2012100982400 A CN 2012100982400A CN 201210098240 A CN201210098240 A CN 201210098240A CN 102600800 A CN102600800 A CN 102600800A
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- Prior art keywords
- adsorbents
- semi
- preparation
- coke
- adsorbent
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000571 coke Substances 0.000 title abstract 5
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000003077 lignite Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000012986 modification Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 abstract description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052740 iodine Inorganic materials 0.000 abstract description 5
- 239000011630 iodine Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract 2
- 235000011007 phosphoric acid Nutrition 0.000 abstract 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Landscapes
- Water Treatment By Sorption (AREA)
Abstract
The invention provides a preparation method of semi-coke adsorbents. The preparation method comprises the steps of: heating brown coal under the condition that air is isolated, preserving heat and cooling to room temperature with a furnace; crushing into particles; and then immersing in H3PO4 solution for H3PO4 modification at constant temperature, washing the modified particles with deionized water and drying to constant weight to obtain the semi-coke adsorbents. The specific surface area of the prepared semi-coke adsorbents reaches 915m<2>/g and the iodine value reaches 800mg/g. According to tests, the removal rate of chemical oxygen demands (COD) in organic tin wastewater reaches 85 percent, the cost is low, the raw materials are sufficient, the preparation process is simple and the yield is high; and the semi-coke adsorbents can replace activated charcoal adsorbents and pollution is not caused.
Description
Technical field
The present invention relates to a kind of semicoke preparation of adsorbent method, belong to adsorbent utilization and preparing technical field.
Background technology
Utilize acticarbon to handle in industrial waste gas, the waste water at present and be most widely used, but active carbon there is cost high, problems such as raw material supplying difficulty.The semicoke adsorbent is the flammable coking product by coal low temperature distillation gained, through the porosu solid adsorbent that processes such as fragmentation, screening, modification obtain, compares with active carbon that it is with low cost, the raw material abundance.The preparation of semicoke adsorbent is mentioned in patent application 201110036170.1 among patent 200410079366.9, the patent application 200610097865.X, but only to the gas absorption reflection that produces effect.The report of pollutant is also very rare in the semicoke adsorbents adsorb liquid phase at present.
Summary of the invention
The present invention is directed to and use pollutant in the semicoke adsorbents adsorb liquid phase, a kind of semicoke preparation of adsorbent method is provided, realize through following technical proposal.
A kind of semicoke preparation of adsorbent method, following each step of process:
(1) with brown coal under the condition of secluding air, be heated to 500～700 ℃, and be incubated 60～120min, cool to room temperature then with the furnace;
(2) brown coal powder after step (1) heating is broken to 5～20 purpose particles;
(3) step (2) gained particle being immersed in volumetric concentration is 30～50% H
3PO
4In the solution, and carry out H in 75～85 ℃ of following constant temperature 180min
3PO
4Modification, the particle after the modification is extremely neutral with deionized water rinsing, and dry to constant weight, promptly obtain the semicoke adsorbent.
Brown coal powder particle after said step (2) is pulverized, and is dried to constant weight with removal fine powder wherein with deionized water rinsing.
Organo-tin compound is one of best heat stabilizer of polyvinyl chloride (PVC), existing at present nearly 60 years production history.Organotin wastewater belongs to the condensation waste water that produces in its production process, and water quality is complicated, and intense stimulus property smell is arranged, and mainly contains a large amount of organic pollutions, belongs to high concentration, poisonous, difficult-degradation organic sewage.Organotin wastewater does not have ripe treatment process temporarily at present, and there are shortcomings such as long flow path, cost height in the organotin processing method of industrial waste water at present.Raw material sources of the present invention are extensive, and price is cheap, and the gained adsorbent has good adsorption property, the semicoke adsorbent of preparing, and its specific area reaches 915m
2/ g, iodine number reaches 800mg/g.Through evidence, be that the COD clearance in the organotin wastewater of 700～750mg/L reaches 85% to COD content, final adsorbent also can be used for boiler oil, non-secondary pollution.
The present invention has the following advantages:
(1) (about 500 yuan/ton) with low cost, raw material is sufficient, and the preparation process is simple, and yield is high;
(2) adsorbents adsorb of gained is effective, and the clearance of COD is very good in experiment showed, organotin wastewater, can substitute acticarbon;
(3) the semicoke adsorbent behind the absorption large amount of organic can be used for boiler combustion, and a large amount of calorific values is provided, and has really realized complete alternation, does not have any secondary pollution;
(4) in the preparation process, there is not any pollution, used H
3PO
4Can reuse through reclaiming;
(5) not only reduced the cost of adsorbent as adsorbent with semicoke; Semicoke has higher calorific value behind the adsorb organic compound, can get into boiler and burn, and directly generates water and carbon dioxide behind the organic compound combustion; Get into smoke dust system; Really realized complete alternation, pollution-free, the target of zero-emission.
The specific embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
(1) with brown coal under the condition of secluding air, be heated to 500 ℃ through Muffle furnace, and the insulation 60min, cool to room temperature then with the furnace;
(2) brown coal powder after step (1) heating is broken to 5～10 purpose particles; Then with deionized water rinsing removing fine powder wherein, and dry to constant weight;
(3) step (2) gained particle being immersed in volumetric concentration is 30% H
3PO
4In the solution, and carry out H in 75 ℃ of following constant temperature 180min
3PO
4Modification, the particle after the modification is extremely neutral with deionized water rinsing, and dry to constant weight, promptly obtain the semicoke adsorbent.
The yield of gained semicoke adsorbent is 72%, and specific area is 924m
2/ g, iodine number is 847mg/g, is that the COD clearance in the organotin wastewater of 700～750mg/L reaches 84.4% to COD content.
Embodiment 2
(1) with brown coal under the condition of secluding air, be heated to 640 ℃ through Muffle furnace, and the insulation 100min, cool to room temperature then with the furnace;
(2) brown coal powder after step (1) heating is broken to 5～10 purpose particles; Then with deionized water rinsing removing fine powder wherein, and dry to constant weight;
(3) step (2) gained particle being immersed in volumetric concentration is 50% H
3PO
4In the solution, and carry out H in 85 ℃ of following constant temperature 180min
3PO
4Modification, the particle after the modification is extremely neutral with deionized water rinsing, and dry to constant weight, promptly obtain the semicoke adsorbent.
The yield of gained semicoke adsorbent is 67%, and specific area is 945m
2/ g, iodine number is 886mg/g, is that the COD clearance in the organotin wastewater of 700～750mg/L reaches 86.4% to COD content.
Embodiment 3
(1) with brown coal under the condition of secluding air, be heated to 700 ℃, and the insulation 120min, cool to room temperature then with the furnace;
(2) brown coal powder after step (1) heating is broken to 10～20 purpose particles; Then with deionized water rinsing removing fine powder wherein, and dry to constant weight;
(3) step (2) gained particle being immersed in volumetric concentration is 40% H
3PO
4In the solution, and carry out H in 80 ℃ of following constant temperature 180min
3PO
4Modification, the particle after the modification is extremely neutral with deionized water rinsing, and dry to constant weight, promptly obtain the semicoke adsorbent.
The yield of gained semicoke adsorbent is 58%, and specific area is 903m
2/ g, iodine number is 834mg/g, is that the COD clearance in the organotin wastewater of 700～750mg/L reaches 83.4% to COD content.
Claims (2)
1. semicoke preparation of adsorbent method is characterized in that through following each step:
(1) with brown coal under the condition of secluding air, be heated to 500～700 ℃, and be incubated 60～120min, cool to room temperature then with the furnace;
(2) brown coal powder after step (1) heating is broken to 5～20 purpose particles;
(3) step (2) gained particle being immersed in volumetric concentration is 30～50% H
3PO
4In the solution, and carry out H in 75～85 ℃ of following constant temperature 180min
3PO
4Modification, the particle after the modification is extremely neutral with deionized water rinsing, and dry to constant weight, promptly obtain the semicoke adsorbent.
2. semicoke preparation of adsorbent method according to claim 1 is characterized in that: the brown coal powder particle after said step (2) is pulverized is used deionized water rinsing, and dries to constant weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100982400A CN102600800A (en) | 2012-04-06 | 2012-04-06 | Preparation method of semi-coke adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100982400A CN102600800A (en) | 2012-04-06 | 2012-04-06 | Preparation method of semi-coke adsorbent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102600800A true CN102600800A (en) | 2012-07-25 |
Family
ID=46518790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100982400A Pending CN102600800A (en) | 2012-04-06 | 2012-04-06 | Preparation method of semi-coke adsorbent |
Country Status (1)
| Country | Link |
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| CN (1) | CN102600800A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691410A (en) * | 2014-01-09 | 2014-04-02 | 中国矿业大学(北京) | Rare-earth modified semicoke coal powder material and preparation method thereof |
| CN105170082A (en) * | 2015-09-09 | 2015-12-23 | 延安大学 | Preparation method of semi-coke adsorbent |
| CN105664892A (en) * | 2016-01-20 | 2016-06-15 | 昆明理工大学 | Method for preparing arsenic adsorbing material by lignite and yellow phosphorus water-quenched slag |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1342880A1 (en) * | 1985-08-08 | 1987-10-07 | Львовский политехнический институт им.Ленинского комсомола | Method of removing organic compounds from tar water of shale-processing production |
| CN101362101A (en) * | 2008-09-11 | 2009-02-11 | 中国海洋大学 | Semi-coke forming SO2and NO adsorptive catalyst and preparation method thereof |
| CN102120178A (en) * | 2011-02-11 | 2011-07-13 | 广东工业大学 | Active semicoke adsorbing agent and preparation method thereof |
-
2012
- 2012-04-06 CN CN2012100982400A patent/CN102600800A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1342880A1 (en) * | 1985-08-08 | 1987-10-07 | Львовский политехнический институт им.Ленинского комсомола | Method of removing organic compounds from tar water of shale-processing production |
| CN101362101A (en) * | 2008-09-11 | 2009-02-11 | 中国海洋大学 | Semi-coke forming SO2and NO adsorptive catalyst and preparation method thereof |
| CN102120178A (en) * | 2011-02-11 | 2011-07-13 | 广东工业大学 | Active semicoke adsorbing agent and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691410A (en) * | 2014-01-09 | 2014-04-02 | 中国矿业大学(北京) | Rare-earth modified semicoke coal powder material and preparation method thereof |
| CN103691410B (en) * | 2014-01-09 | 2015-09-30 | 中国矿业大学(北京) | rare earth modified semicoke coal powder material and preparation method thereof |
| CN105170082A (en) * | 2015-09-09 | 2015-12-23 | 延安大学 | Preparation method of semi-coke adsorbent |
| CN105664892A (en) * | 2016-01-20 | 2016-06-15 | 昆明理工大学 | Method for preparing arsenic adsorbing material by lignite and yellow phosphorus water-quenched slag |
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Application publication date: 20120725 |