CN1178854C

CN1178854C - Method for producing active carbon from coal water mixture

Info

Publication number: CN1178854C
Application number: CNB021280398A
Authority: CN
Inventors: 肖仁贵; 曾祥钦; 李宜芳; 廖霞; 朱静
Original assignee: GUIZHOU POLYTECHNICAL UNIV
Current assignee: GUIZHOU POLYTECHNICAL UNIV
Priority date: 2002-12-12
Filing date: 2002-12-12
Publication date: 2004-12-08
Anticipated expiration: 2022-12-12
Also published as: CN1415539A

Abstract

The present invention relates to a method for manufacturing active carbon by water coal slurry. The present invention is realized through the steps: lignin is added in the process of manufacturing coal water slurry by coal; then, active carbon is obtained after the coal water slurry with lignin is orderly treated by the steps of pretreating by acid, drying, shaping, carbonizing, activating, recovering activating agent, rinsing, drying and grinding. Compared with the prior art, the present invention has no specific requirements to the quality of coal, and enormous coal resources in China can be utilized as raw materials, so the source of raw materials for producing active carbon is enlarged, and the productive cost of active carbon is lowered thereby; the adsorbability of active carbon from coal can be enhanced because of the addition of lignin; good quality active carbon of which the iodine value can reach over 1500 mg/g can be obtained.

Description

Make process of active carbon with coal water slurry

Technical field: the present invention relates to the production method of gac, particularly make process of active carbon with coal water slurry.

Prior art: gac is widely used in the gac in fields, particularly high absorption property such as environmental protection, catalyzer, gas and water purification, and its application prospect is more considerable; The raw material of the gac of China's production at present mainly contains wooden (comprising shell) and ature of coal two classes, because the general forestry processing waste materials of using of gac are produced in China's forest resourceies shortage more; Along with the minimizing day by day of the forest reserves, wood materials is originated fewer and feweri, will the manufacturing cost of gac be increased; Coal resources in China is abundanter, and coal production ranks first in the world, but is used to produce the resource of the low ash content of gac, weak type of bond and few, China's not somatotype exploitation at present in addition, and the coal mass active carbon raw material can be more and more nervous; In addition, in the prior art, the production of carrying out gac with raw coal generally is directly to process, because the ash content of coal is big in the coal, carbon crystalline network degree height has influenced the absorption property of institute's preparing active carbon, so its quality product is poorer than the gac of producing with wood materials, the product absorption property is lower, and its iodine number is generally below 1000mg/g.

The purpose of this invention is to provide a kind of manufacturing process of active carbon, particularly make process of active carbon with the coal water slurry of having added the some amount xylogen; The product absorption property height that this method is made, good product quality does not have special requirement to the raw coal that uses in producing simultaneously, has enlarged like this and has produced the raw material sources of gac, and can make high grade activated carbon, compares with wood material and will reduce production costs.

The present invention is achieved in that to make in the process of coal water slurry of coal and adds xylogen, and then carries out sour pre-treatment, drying and moulding, charing, activation, recovery activator, rinsing, drying, grinding and obtain gac; Among the present invention, the coal that the system coal water slurry is used and the weight ratio of xylogen are 1: 0.1～3.Specifically, coal grinding is become powder, sieve, coal dust and xylogen are mixed after the weighing in proportion, and the container of packing into adds entry, make coal water slurry after the stirring, add the acid solution that the perchloric acid by equivalent weight becomes with mixed in hydrochloric acid, after stirring, place, be washed with water to neutrality, natural air drying then, add potassium hydroxide again and mix, add less water, stir, put into activation furnace activation,

Charing under nitrogen protection, is warming up to 700-900 degree Celsius and insulation by the heat-up rate of 5～10 ℃/min, after the cooling, with the activation products fragmentation, adds the salt acid soak, is washed with water to neutrality, use oven for drying, and levigate screening must activated carbon product; More particularly, can produce like this: (1) becomes powder to coal grinding, crosses 200 purpose sieves; (2) coal dust and xylogen are weighed the container of packing in the ratio of 1: 0.1～3 (weight ratios); (3) water of adding 8% is made coal water slurry after the stirring; (4) add 1: 1 37% perchloric acid and 36.5% hydrochloric acid, after stirring, placed 24 hours; (5) be washed with water to after pH is 6 natural air drying; (6) added potassium hydroxide by weight 1: 1 and mix, add less water, stir; (7) put into activation furnace activation charing, under nitrogen protection, be warming up to 800 ℃, be incubated 1 hour by the heat-up rate of 5～10 ℃/min; (8) after the cooling,, added the salt acid soak 1 hour with the activation products fragmentation; (9) being washed with water to pH is 6, uses oven for drying, and levigate screening gets activated carbon product.

Compared with prior art, because the present invention does not have particular requirement to the quality of coal, can utilize the coal resources of China's abundant to make raw material, thereby enlarged the source that produces the gac raw material, and reduce the production cost of gac thus, the adding xylogen can improve the absorption property of active carbon from coal, makes iodine number and can reach the above high grade activated carbon of 1500mg/g.

Embodiments of the invention 1: get the 2kg coal cinder at random, with PE-60 * 100 jaw crusher coarse crushings, with OM-4H type ball mill particulate coal is carried out fine grinding again, coal dust is crossed 200 mesh sieve, take by weighing the coal dust 100g after sieving, take by weighing xylogen 45g in addition, stir, add 100mL water, make coal water slurry, coal water slurry is put into beaker, add hydrochloric acid (36.5%) 15mL, perchloric acid (37%) 15mL, after stirring, place 24h, it is about 6 that coal water slurry after the above-mentioned acid treatment is washed with water to pH, with electrically heated drying cabinet water is dried, take by weighing above-mentioned oven dry thing 10g, add activator KOH10g, water 6mL stirs, be transferred in the porcelain boat, porcelain boat is put into the stainless-steel pipe middle part, again stainless-steel pipe is put into electric tube furnace, in whole heat-processed, feed industrial nitrogen; Open the nitrogen valve; the adjustments of gas flow is 1.0L/min; connect power supply then, use the transformer regulating voltage, making the tube type resistance furnace heat-up rate is 8 ℃/min; when temperature rises to 800 ℃; be incubated 30 minutes, powered-down is cooled to room temperature under nitrogen protection; close the nitrogen valve; take out activated carbon product, put into beaker, add dilute hydrochloric acid solution 20mL; soaked 30 minutes; being washed with water to pH is 6, and drying gets gac 6.2g; the gac that this method makes is measured iodine number by method shown in the GB/T 7702.7-1997, be 1200mg/g.

Embodiments of the invention 2: get the 2kg coal cinder at random, with PE-60 * 100 jaw crusher coarse crushings, with OM-4H type ball mill particulate coal is carried out fine grinding again, coal dust is crossed 200 mesh sieve, take by weighing the back coal dust 60g that sieves, take by weighing xylogen 140g in addition, stir, add 150mL water, make coal water slurry, coal water slurry is put into beaker, add hydrochloric acid (36.5%) 20mL, perchloric acid (37%) 20mL, after stirring, place 24h, coal water slurry after the above-mentioned acid treatment is washed with water to neutrality, water is dried with electrically heated drying cabinet, take by weighing above-mentioned oven dry thing 10g, add activator KOH 10g, water 6mL stirs, be transferred in the porcelain boat, porcelain boat is put into the stainless-steel pipe middle part, again stainless-steel pipe is put into electric tube furnace, in whole heat-processed, feed industrial nitrogen; Open the nitrogen valve; the adjustments of gas flow is 1.0L/min; connect power supply then, use the transformer regulating voltage, making the tube type resistance furnace heat-up rate is 5 ℃/min; when temperature rises to 700 ℃; be incubated 30 minutes, powered-down is cooled to room temperature under nitrogen protection; close the nitrogen valve; take out activated carbon product, put into beaker, add dilute hydrochloric acid solution 20mL; soaked 30 minutes; be washed with water to neutrality, drying, use gac 5g; the gac that this method makes is measured iodine number by method shown in the GB/T 7702.7-1997, be 1320mg/g.

Embodiments of the invention 3: get the 2kg coal cinder at random, with PE-60 * 100 jaw crusher coarse crushings, with OM-4H type ball mill particulate coal is carried out fine grinding again, coal dust is crossed 200 mesh sieve, take by weighing the back coal dust 100g that sieves, take by weighing xylogen 100g in addition, stir, add 150mL water, make coal water slurry, coal water slurry is put into beaker, add hydrochloric acid (36.5%) 20mL, perchloric acid (37%) 20mL, after stirring, place 24h, it is about 6 that coal water slurry after the above-mentioned acid treatment is washed with water to pH, with electrically heated drying cabinet water is dried, take by weighing above-mentioned oven dry thing 10g, add activator KOH10g, water 6mL stirs, be transferred in the porcelain boat, porcelain boat is put into the stainless-steel pipe middle part, again stainless-steel pipe is put into electric tube furnace, in whole heat-processed, feed industrial nitrogen; Open the nitrogen valve, the adjustments of gas flow is 1.0L/min, connects power supply then, use the transformer regulating voltage, making the tube type resistance furnace heat-up rate is 8 ℃/min, when temperature rises to 900 ℃, be incubated 60 minutes, powered-down is cooled to room temperature under nitrogen protection, close the nitrogen valve, take out activated carbon product, put into beaker, add dilute hydrochloric acid solution 20mL, soaked 30 minutes, being washed with water to pH is 6, kept dry gets gac 4.2g; The gac that this method makes is measured iodine number by method shown in the GB/T 7702.7-1997, be 1580mg/g.

Claims

1, a kind ofly makes process of active carbon with coal water slurry; it is characterized in that: produce coal water slurry with coal; mix after in making the process of coal water slurry, coal dust and xylogen being 1: 0.1～3 weighings by weight; make coal water slurry after the stirring; and then add the acid solution that the perchloric acid by equivalent weight becomes with mixed in hydrochloric acid and carry out pre-treatment, drying and moulding, put into that activation furnace activates, charing: under nitrogen protection; heat-up rate by 5～10 ℃/min is warming up to 700-900 degree Celsius and insulation, and recovery activator, rinsing, drying, grinding obtain gac.

2, make process of active carbon according to claim 1 is described with coal water slurry, it is characterized in that: in preparation coal water slurry process, at first coal grinding is become powder, sieve; In coal water slurry, add the acid solution that the perchloric acid by equivalent weight becomes with mixed in hydrochloric acid, after stirring, place, be washed with water to neutrality, natural air drying then, add potassium hydroxide again and mix, add less water, stir, put into that activation furnace activates, charing; Activated, charing postcooling in the activation furnace with the activation products fragmentation, adds the salt acid soak, is washed with water to neutrality, uses oven for drying, and levigate screening gets activated carbon product.