CN106395816A - Method for extracting humic acid from lignite and then using residues to prepare adsorbent - Google Patents

Method for extracting humic acid from lignite and then using residues to prepare adsorbent Download PDF

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CN106395816A
CN106395816A CN201610800830.1A CN201610800830A CN106395816A CN 106395816 A CN106395816 A CN 106395816A CN 201610800830 A CN201610800830 A CN 201610800830A CN 106395816 A CN106395816 A CN 106395816A
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pyrolysis
coal
humic acid
gas
lignite
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CN106395816B (en
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杨小芹
张双全
岳晓明
朱凯文
赫帅
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China University of Mining and Technology CUMT
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    • 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
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

Abstract

The invention discloses a method for extracting humic acid from lignite and then using residues to prepare an adsorbent. An alkali dissolution and acid precipitation method is adopted to extract humic acid from lignite, pyrolysis is conducted on the residues at the temperature of 760-940 DEG C, a pyrolysis gas product is condensed and cooled to prepare tar and hydrogen-rich gas, a pyrolysis solid product is washed and dried to prepare a carbonaceous adsorbent, and graded conversion and utilization of the lignite are achieved. According to the method, the alkali liquor in the residues after the humic acid is extracted from the lignite is utilized, the carbonaceous adsorbent having large specific surface area and good adsorption property is prepared through high-temperature pyrolysis in a one-step mode, and the shortcomings of large alkali amount, complicated process and high cost of a traditional process for preparing activated carbon based on an alkali activation method are overcome. A byproduct tar contains little pyrolysis water, is easy to separate, high in yield, a byproduct raw coal gas has very high H2 and CO content, the CH4 content is low, and the produced gas serves as chemical raw gas after being purified and modified.

Description

A kind of method that after extracting humic acidss by brown coal, residue prepares adsorbent
Technical field
The present invention relates to a kind of coal comprehensive utilization technique, residue preparation after specifically a kind of extracting humic acidss by coal The method of adsorbent.
Background technology
With a large amount of exploitations of coal, China's high-quality coal resource gradually decreases, but lignite resource enriches underutilization, Efficient utilization is carried out to the lignite resource of rich reserves there is very high economy and social value.Therefore, brown coal are effectively improved Comprehensively utilize and develop towards high value added product direction and be increasingly becoming study hotspot.
Brown coal are that a kind of high volatile, high-moisture, high ash, low heat value, low ash smelting point, chemical reactivity are strong, thermally-stabilised Property is poor, easy-weathering fragmentation, the inferior fuel of oxidizable spontaneous combustion, be the minimum coal of degree of coalification.Directly by brown coal burning wave completely Oil, gas and the chemicals in brown coal with high added value are taken.The pyrolysis of coal is the important production technology of coal hot-working aspect, Coal is in isolation air（Or inert atmosphere）Under conditions of, low temperature pyrogenation（500～700 DEG C）The coal tar of high yield can be obtained Oily, middle warm solution（700～1000 DEG C）The coal gas of high yield, high temperature pyrolysis can be obtained（1000～1200 DEG C）Obtain high-quality The coke of amount.Domestic pyrolysis using brown coal in a large number at present carries out brown coal upgrading, liquefaction and gas processed with technology such as brown coal dry distilling, for example Chinese invention patent application file《Low-order coal classified utilization polygenerations systeme and method》（Publication number CN105154121A, patent Application number 201510665313.3）, low-order coal is carried out the quick dry distilling of low temperature and processes, obtain raw coke oven gas, tar and semicoke, coal tar Oil is hydrogenated with acquisition oil product further, and raw coke oven gas obtains coal gas through purified treatment, and semicoke is supplied gas fluidized bed gasification.But utilize brown coal It is pyrolyzed the research of adsorbent processed and technology has no report.
Chinese invention patent application file《Municipal sludge and agricultural wastes oil producing technology for co-pyrolysis》（Publication number CN101643687, application number 200910184253.8）Propose, the mixture pyrolysis to municipal sludge and agricultural wastes（400 ～750 DEG C）, can get oil, water-soluble liquid and incoagulability fuel gas；Pyrolysis solid product is carried out grinding can be used as activity Carbon adsorbent.But, the acticarbon hole that this method obtains is undeveloped, and specific surface area and pore volume are little.Generally activity The preparation of charcoal needs through carbonization and two stages of activation, and wherein activation process is the most key.Activation mainly point physically activated and Chemical activation, widely uses KOH activator activation ature of coal or coke raw material in chemical activation method.But activate presence alkali with alkali Amount is big（Alkali coke ratio is about 3：1～4：1）, complex process, the problem of high cost.
Additionally, original humic acid is brown coal being different from the principal character component of other coals.Alkali density brown coal produce humic Acid is important directions of brown coal comprehensive utilization.Humic acid is widely used to the fields such as metallurgy, chemical industry, agricultural, environmental protection.So And after extracting brown coal residue using rarely having research.In humic acid manufacturer, using conventional caustic extraction method by coal After middle humic acid dissolution, remaining residue is typically discharged as solid refuse.Also contain one in addition to containing inorganic substances in residue Quantitative organic matter, discharges this residue, causes the negative influences such as environmental pollution and the wasting of resources as solid refuse.
Chinese invention patent application file《A kind of stepped utilization method of poor quality brown coal》（Publication number CN104987873A, Number of patent application 201510269565.4）Propose, brown coal inferior are first carried out humic acid extraction, the brown coal residue being subsequently dried It is pyrolyzed, produced semicoke, tar and raw gas.By humic acid-extraction step, on the one hand obtain having more extensively applying The humic acid of scope, simultaneously because the extraction of humic acid, reduces oxygen content in brown coal, and the interior water thus reducing in coal is divided with coal The hydrogen bond existing between son, contributes to the dried of brown coal.Secondly, the low oxygen content brown coal residue having extracted humic acid is used for Pyrolytic process, prepares lignite semi-coke, tar and raw gas.Technology disclosed in this document, the pyrolysis temperature to brown coal residue is 400 ～750 DEG C, belong to low temperature pyrogenation.The added value of pyrolysis gained solid product semicoke is low, does not truly realize brown coal Efficient cascade utilization.
Content of the invention
The technical problem to be solved in the present invention is, overcomes the defect that prior art exists it is proposed that one kind is taken out by brown coal The method that after carrying humic acidss, residue prepares adsorbent.With Lignitic Humic Acid extraction-high temperature pyrolysis as main technological route, to brown coal Carry out staged conversion utilization, i.e. extracted humic acid, residue is pyrolyzed carbonaceous adsorbent processed, by-product tar and hydrogen-rich gas.Using coal Liquid base in residue after the extraction of charcoal humic acid, one-step method prepares Cheap highly effective adsorbent, overcomes traditional alkali activation legal system In standby activated carbon process, alkali charge is big（Alkali coke ratio is about 3：1～4：1）, complex process, the problem of high cost.
The present invention solves technical problem, and the basic ideas realizing goal of the invention are：Extract coal in conventional alkali-soluble acid analysis method After middle humic acid, solid residue is carried out with high temperature pyrolysis, prepared high-performance low-cost sorbent, by-product tar and hydrogen-rich gas.
The technical scheme of solve problem of the present invention, extracts, by brown coal, the method that after humic acidss, residue prepares adsorbent, including Following steps：
Step one, brown coal are dried, crush, remove impurity, screening, take 40 mesh siftage（Coal dust）.
Step 2, coal dust is added in the aqueous slkali that mass percent concentration is 2～6%, water at a temperature of 50～90 DEG C Bath heating 0.5～3h, obtains reacted mixture.Coal dust is 1 with the mass ratio of aqueous slkali：20～1：100.
Step 3, by reacted mixture cool down after centrifugation, leach the supernatant, after acid out obtain humic acid, Precipitate after centrifugation is the residue after extracting humic acidss..
Step 4, will extracting humic acidss after precipitate 105～120 DEG C dry, in pyrolysis oven completely cut off air or lazy Property gas shield under, heat up pyrolysis, pyrolysis final temperature be 760～940 DEG C, constant temperature time 0.5～4h.
Step 5, pyrolysis gas product is carried out condensation cooling, you can obtain oil water mixture and hydrogen-rich gas, profit mix Compound can be further processed into useful downstream product.
Step 6, the solid matter with deionized water after pyrolysis is washed to neutrality, and high temperature is dried to constant weight, finally obtains Obtain carbonaceous adsorbent.Said high temperature, the present invention is not particularly limited to temperature, and those skilled in the art are according to basic general knowledge Design temperature carries out drying to the solid product after pyrolysis.Described constant weight, does not have special weighting error index to limit, heat yet Solid product after solution is dried to meeting adsorbent use.
The present invention is to realize goal of the invention, and further improved technical scheme is：Described step 2, coal dust is pre-oxidized after It is added to heating in water bath in aqueous slkali, obtain reacted mixture.Described coal dust method for pre-oxidizing is that coal dust is added quality Percent concentration is 5～18%HNO3In solution, solid-liquid mass ratio（Coal dust and salpeter solution mass ratio）For 1:4～1：8,50 Heating in water bath 0.5～2h at a temperature of～90 DEG C, cooling, filtration washing is to neutrality.
In step 2, described aqueous slkali can be NaOH, Na2CO3、Na2P2O7One or more of solution mixture.
The principle of the present invention：Humic acid in brown coal is extracted using traditional alkali-soluble acid analysis method, alkali is in extracted humic acid process In destroy Ar-O-C oxygen-containing functional group in coal, this effect one side contributes to the dried of brown coal, on the other hand big Decrease greatly the generation being pyrolyzed water in brown coal residue pyrolytic process, reduce the separating difficulty of oil water mixture, improve simultaneously The quality of tar.In residue, the alkali of residual serves the effect of activation reaming in pyrolytic process to semicoke, and this effect is main It is to occur at high temperature, so that the absorption property of Jiao is increased substantially.High temperature is the essential condition of activation pore-creating.Meanwhile, alkali With-CH in coal2- and-CH- and semicoke react activation pore-creating while promote more gas evolutions, increased aerogenesis Amount, H in aerogenesis2Significantly improve with the content of CO.The present invention is by above staged conversion method, it is possible to obtain humic acid, carbonaceous Adsorbent, tar and raw gas product.The inventive method is with Lignitic Humic Acid extraction-high temperature pyrolysis as main technological route, right Brown coal carry out staged conversion utilization, i.e. extracted humic acid, and residue is pyrolyzed carbonaceous adsorbent processed, by-product tar and hydrogen-rich gas.Profit Alkali liquor in residue after being extracted with coal humic acid, one-step method high temperature pyrolysis prepare the carbon that specific surface area is high, absorption property is good Matter adsorbent, overcoming traditional alkali activation method, to prepare alkali charge in activated carbon process big（Alkali coke ratio is about 3：1～4：1）, Complex process, the problem of high cost.In the inventive method, to contain pyrolysis water few for the tar of by-product, separates easily, tar yield is high, The raw gas of by-product has very high H2With CO content, CH4Content is low, is highly suitable as chemical industry former after the purified modification of aerogenesis Material gas.
Brief description
Fig. 1 the inventive method process flow diagram.
Specific embodiment
With reference to specific embodiment, the inventive method is described in further detail, but the present invention is not subject to following realities Apply the restriction of example.
Embodiment 1
Humic acid extracts：
With air dried Xianfeng Brown as raw material, carry out pulverization process, remove impurity using coal pulverizer, screening takes 40 mesh siftage （Coal dust）Sealing is collected.Table 1 is the composition analysis of Xianfeng Brown.
Table 1 Xianfeng Brown Industrial Analysis, elementary analysiss
Weigh 5 parts of quality 5g coal samples in there-necked flask, being separately added into 150mL mass percent concentration is 2%, 3%, 4%, 5%, 6% NaOH solution in, heating in water bath 3h, 2.5h, 2h, 1h, 0.5h at 90 DEG C, 80 DEG C, 70 DEG C, 60 DEG C, 50 DEG C respectively.Will be anti- Centrifugation after solution cooling after answering, takes the supernatant to boil off moisture, as humate.Corruption under Different Alkali extracting concentration Grow hydrochlorate yield as shown in table 2.It can be seen that being the humate yield highest obtaining when 4% with NaOH concentration.
Table 2 humate yield
Concentration of lye % 2 3 4 5 6
Humate yield % 13.2 14.5 18.8 18.7 15.9
In embodiment 1,5 parts of coal samples, can first be pre-oxidized, that is,：It is 5～18% that coal dust is added mass percent concentration HNO3In solution, solid-liquid mass ratio（Coal dust and salpeter solution mass ratio）For 1:4～1：8, water-bath at a temperature of 50～90 DEG C adds Hot 0.5～2h, cooling, filtration washing is to neutrality.
Embodiment 2
Pyrolysis：
Weigh 40～80 mesh air dried Xianfeng Brown 5g, concentration be 4% 150mLNaOH solution at 80 DEG C water-bath add Hot 1h.Centrifugation after reacted solution is cooled down, precipitate is put into 105 in baking ovenoC is dried 2h.Weigh 3g drying brown coal Residue is put in pyrolytic reaction pipe, and logical nitrogen does shielding gas, and the heating rate of design temperature controller is 10oC/min, respectively 760oC and 940oC is pyrolyzed final temperature（Also known as pyrolysis temperature in embodiment）Lower pyrolysis, constant temperature time 30 min.After pyrolysis Solid matter with deionized water is washed to neutrality, and high temperature is dried to constant weight, finally obtains described carbonaceous adsorbent.
Through actual experiment checking, drying brown coal residue completely cuts off under air or inert gas shielding in pyrolysis oven, rises warm Solution, pyrolysis final temperature, between 760～940 DEG C, all can obtain described carbonaceous adsorbent between constant temperature time 0.5～4h, realizes Goal of the invention.
In order to be contrasted, weigh 40～80 mesh base Xianfeng Brown 3g is dried and be pyrolyzed in the same way.Table 3 is heat Solution gained factor of created gase and aerogenesis composition, table 4 is iodine number, specific surface area, pore volume and the average pore size of gained solid product.
Table 3 pyrolysis factor of created gase and aerogenesis composition
As can be seen from the above table, the factor of created gase of brown coal residue is more than the factor of created gase of raw coal.The presence of alkali is described, and to promote brown coal residual The orientation conversion of slag pyrolysis.Brown coal residue is pyrolyzed the content up to more than 30% of CO in aerogenesis composition, (H2+ CO) content 900o78% is reached, than (the H of brown coal pyrolysis under the same terms during C pyrolysis2+ CO) content high by 14.5%.The high warm of brown coal residue is described The aerogenesis that solution obtains is more suitable for as chemical industry synthesis gas.Higher CO content also illustrate that NaOH sends out in pyrolytic process simultaneously Give birth to activation.
The iodine number of solid product and pore structure parameter under the different pyrolysis temperature of table 4
As can be seen from the above table, the solid product iodine number that Xianfeng Brown pyrolysis obtains is relatively low, the solid that brown coal residue pyrolysis obtains Product adsorbance dramatically increases, and this difference is 900oParticularly evident during C, illustrate that NaOH plays good activation in high temperature Reaming acts on.Additionally, the N from semicoke2It is burnt burnt with Xianfeng Brown pyrolysis that adsorption/desorption isotherms can be seen that brown coal residue pyrolysis Compare and have more abundant mesopore.Brown coal residue 900oThe pyrogenically prepared active carbocoal of C is 612.4 m than table2/ g, pore volume reaches 0.3928 cm3/ g, can use as adsorbent.
Embodiment 3
Weigh below 80 mesh air dried Xianfeng Brown 5g, be separately added into concentration be 2%, 3%, 4%, 5% 300mLNaOH solution In, 50oUnder C, ultrasonic water bath heats 20 min.Centrifugation after reacted solution is cooled down, precipitate is put in baking oven 105oC is dried 2 h.Weigh 3g drying brown coal residue and put in pyrolytic reaction pipe, logical nitrogen does shielding gas, design temperature controls The heating rate of device is 10oC/min, 900oIt is pyrolyzed under C pyrolysis temperature, constant temperature time is 20 min.Table 5 is that Different Alkali is dense The burnt iodine number of brown coal residue pyrolysis, specific surface area, pore volume and average pore size after degree extracting humic acid.
The different alkali concn of table 5 extracts the burnt iodine number of residue pyrolysis and pore structure parameter after Lignitic Humic Acid
NaOH concentration/% Iodine number/(mg/g) Specific surface area/（m2/g） Pore volume/（cm3/g） Average pore size/nm
3 666.7 497.5 0.2777 2.233
5 845.0 707.0 0.4970 2.812
Embodiment 4
Substantially the same manner as Example 3, except that aqueous slkali is Na2CO solution.
Embodiment 5
Substantially the same manner as Example 3, except that aqueous slkali is NaOH and Na2P2O7Mixture.

Claims (4)

1. a kind of method that after extracting humic acidss by brown coal, residue prepares adsorbent, comprises the following steps：
Step one, brown coal are dried, crush, remove impurity, screening, take coal dust under 40 mesh sieves；
Step 2, coal dust is added in aqueous slkali, heating in water bath, obtains reacted mixture；
Step 3, by reacted mixture cool down after centrifugation, leach the supernatant, after acid out obtain humic acid, centrifugation Precipitate afterwards is the residue after extracting humic acidss；
Step 4, will extracting humic acidss after precipitate dry after, in pyrolysis oven isolation air or inert gas shielding under, rise Warm solution, pyrolysis final temperature is 760～940 DEG C, constant temperature time 0.5～4h；
Step 5, pyrolysis gas product is carried out condensation cooling, obtain oil water mixture and hydrogen-rich gas；
Step 6, the solid matter with deionized water after pyrolysis is washed to neutrality, and dry to constant weight, obtain carbonaceous absorption Agent.
2. the method that after the extracting humic acidss by brown coal according to claim 1, residue prepares adsorbent, is characterized in that：Described Step 2, coal dust is pre-oxidized after be added to heating in water bath in aqueous slkali, obtain reacted mixture；Described coal dust pre-oxidation Method is that coal dust is added mass percent concentration is 5～18%HNO3In solution, coal dust and salpeter solution mass ratio are 1:4～ 1：8, heating in water bath 0.5～2h at a temperature of 50～90 DEG C, cooling, filtration washing is to neutrality.
3. the method that after the extracting humic acidss by brown coal according to claim 1 and 2, residue prepares adsorbent, is characterized in that： The mass percent concentration of aqueous slkali described in step 2 is 2～6%, and the temperature of heating in water bath is 50～90 DEG C, and heat time heating time is 0.5 ~ 3h, coal dust is 1 with the mass ratio of aqueous slkali：20～1：100.
4. the method that after the extracting humic acidss by brown coal according to claim 3, residue prepares adsorbent, is characterized in that：Step In two, described aqueous slkali is NaOH, Na2CO3、Na2P2O7One or more of solution mixture.
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Cited By (7)

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CN110615437A (en) * 2019-09-28 2019-12-27 内蒙古科技大学 Comprehensive utilization method of lignite
CN110615436A (en) * 2019-09-27 2019-12-27 内蒙古科技大学 Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues
CN111574006A (en) * 2020-05-31 2020-08-25 佛山经纬纳科环境科技有限公司 Method for recovering catalytic pyrolysis resources of oily sludge
CN112827475A (en) * 2020-12-30 2021-05-25 东北农业大学 Preparation method and application of artificial humic acid functionalized colloid-like magnetic biochar
CN114957702A (en) * 2022-04-26 2022-08-30 常州大学 Preparation method of high-activity humic acid
CN114956873A (en) * 2022-06-15 2022-08-30 上田环境修复有限公司 Co-production process of rice straw-based potassium humate and activated carbon
CN116705517A (en) * 2023-06-08 2023-09-05 太原理工大学 Porous carbon prepared from lignite as raw material and preparation method and application thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110615436A (en) * 2019-09-27 2019-12-27 内蒙古科技大学 Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues
CN110615437A (en) * 2019-09-28 2019-12-27 内蒙古科技大学 Comprehensive utilization method of lignite
CN111574006A (en) * 2020-05-31 2020-08-25 佛山经纬纳科环境科技有限公司 Method for recovering catalytic pyrolysis resources of oily sludge
CN112827475A (en) * 2020-12-30 2021-05-25 东北农业大学 Preparation method and application of artificial humic acid functionalized colloid-like magnetic biochar
CN114957702A (en) * 2022-04-26 2022-08-30 常州大学 Preparation method of high-activity humic acid
CN114956873A (en) * 2022-06-15 2022-08-30 上田环境修复有限公司 Co-production process of rice straw-based potassium humate and activated carbon
CN116705517A (en) * 2023-06-08 2023-09-05 太原理工大学 Porous carbon prepared from lignite as raw material and preparation method and application thereof

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