CN105186001A - High-adsorbability modified lignin preparation method - Google Patents

High-adsorbability modified lignin preparation method Download PDF

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Publication number
CN105186001A
CN105186001A CN201510356146.4A CN201510356146A CN105186001A CN 105186001 A CN105186001 A CN 105186001A CN 201510356146 A CN201510356146 A CN 201510356146A CN 105186001 A CN105186001 A CN 105186001A
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CN
China
Prior art keywords
lignin
solution
quality
modified
pure water
Prior art date
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Pending
Application number
CN201510356146.4A
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Chinese (zh)
Inventor
周燕
方明学
巩春侠
赵冬冬
陈艳娟
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Tianneng Group Jiangsu Technology Co Ltd
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Tianneng Group Jiangsu Technology Co Ltd
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Priority to CN201510356146.4A priority Critical patent/CN105186001A/en
Publication of CN105186001A publication Critical patent/CN105186001A/en
Pending legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/06—Lead-acid accumulators
    • 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
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4837—Lignin
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Manufacturing & Machinery (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention discloses a high-adsorbability modified lignin preparation method, which comprises: dissolving a proper amount of lignin in an alkaline aqueous solution, and stirring until completely dissolving; heating while stirring, slowly adding a certain amount of hydrogen peroxide, concentrated sulfuric acid and Na2SO3 to the solution, continuously stirring until achieving the required time, stopping the stirring, and carrying out standing cooling; and after the temperature of the solution is recovered to a room temperature, carrying out suction filtration, collecting the filtration residue, filtering, drying, grinding, and screening. According to the present invention, the lignin with characteristics of being used by many manufacturers, low price and not good low temperature performance is selected to be modified, such that advantages of simpleness, feasibility, no pollution and low cost are provided; and the modified lignin has characteristics of large specific surface area, easy dispersion, strong Pb<2+> adsorption, low solubility and the like, can be adopted as the lead-acid battery negative electrode additive, can further be used as the adsorbent for the heavy metal ion Pb<2+> in the sewage, and provides the prominent effect.

Description

A kind of preparation method of high adsorption modified lignin
Technical field
The present invention relates to lead-acid battery additive and sewage disposal absorbent fields, be specifically related to a kind of preparation method of high adsorption modified lignin.
Background technology
Lignin and derivative thereof bear the important organic additive of plate as battery, a certain amount of lead ion can be adsorbed, effectively prevent the contraction on negative plate surface and delay the generation of negative pole lead sulfate passivation, Be very effective in the cryogenic property improving battery, therefore gains great popularity.In addition, lignin class material, owing to having certain adsorptivity and low price, is therefore also widely used at the sewage treatment area containing heavy metal ion.Due to the difference in lignin and derivative processing technology thereof, source, between different lignin class material there is certain gap in physical property, therefore causes its Adsorption of Heavy Metal Ions all can be different or affect aspect to battery performance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high adsorption modified lignin, and simple possible, pollution-free, cost is low, and it is large that modified lignin has specific area, is easy to dispersion, to Pb 2+the features such as adsorptivity is strong, dissolubility is low, it is more outstanding as field effects such as sewage heavy metal treatment agent and battery cathode additives.
The present invention is achieved through the following technical solutions:
A preparation method for high adsorption modified lignin, comprises the following steps:
(1) NaOH getting pure water quality 1-2% is dissolved in proportionaling alkali-forming solution in pure water;
(2) lignin getting pure water quality 3-5% adds in aqueous slkali, is stirred to lignin and dissolves completely;
(3) then step (2) solution is heated with stirring to 40 ~ 60 DEG C, gets H 2o 2slowly add, H 2o 2volume and lignin quality, than V:W=0.3 ~ 0.6, after in reaction 1-2min, are got 98% concentrated sulfuric acid and are slowly added, H 2sO 4volume and lignin quality, than V:W=0.25 ~ 0.4, continue stirring until solution and form homogeneous solution;
(4) Na that quality is lignin quality 40% ~ 70% is got 2sO 3, add in the mixed solution of step (3), and constantly stir, after sustained response 80 ~ 100min, stop heating and stir, leaving standstill cooling;
(5) after step (4) solution is cooled to room temperature, carry out suction filtration, collect filter residue, with pure water by filter residue washing and filtering, drying, grind, sieve, obtain high adsorption modified lignin.
Beneficial effect of the present invention:
The present invention selects a kind of lignin bad by the use of a lot of producers, low price, cryogenic property to carry out modification to it, and simple possible, pollution-free, cost is low; It is large that modified lignin has specific area, is easy to dispersion, to Pb 2+the features such as adsorptivity is strong, dissolubility is low, both can use as lead-acid battery cathode additive, again can as heavy metal ions in sewage Pb 2+adsorbent use, effect is more outstanding.
Accompanying drawing explanation
Fig. 1 is that the modified lignin of lignin and embodiment 1,2,3 is before modified scattered in phenomenon figure in water respectively.
Fig. 2 is the modified lignin absorption figure at different temperatures of lignin and embodiment 1,2,3 before modified.
Embodiment
Embodiment 1
4g lignin is added in the 100g aqueous slkali containing 1gNaOH, after fully dissolving, be heated to 60 DEG C, add 2mlH 2o 2reaction 2min, then slowly adds the dense H of 1ml 2sO 4, be stirred to dissolution homogeneity, in the most backward system, add 2gNa 2sO 3, after reaction 80min, stopping heating and stirring, leave standstill and be cooled to room temperature, carry out suction filtration, collect filter residue, with pure water, filter residue being rinsed 2-3 all over being placed on 130 DEG C of freeze-day with constant temperature, ground 100-200 mesh sieve, then be placed in 50-60 DEG C of oven dry, collection sample.
Embodiment 2
4g lignin is added in the 100g aqueous slkali containing 2gNaOH, after fully dissolving, be heated to 50 DEG C, add 2.4mlH 2o 2, then slowly add the dense H of 1.2ml 2sO 4, be stirred to dissolution homogeneity, in the most backward system, add 1.2gNa 2sO 3, after reaction 90min, stopping heating and stirring, leave standstill and be cooled to room temperature, carry out suction filtration, collect filter residue, with pure water, filter residue being rinsed 2-3 all over being placed on 130 DEG C of freeze-day with constant temperature, ground 100-200 mesh sieve, then be placed in 50-60 DEG C of oven dry, collection sample.
Embodiment 3
4g lignin is added in the 100g aqueous slkali containing 2gNaOH, after fully dissolving, be heated to 70 DEG C, add 2mlH 2o 2, then slowly add the dense H of 1.6ml 2sO 4, be stirred to dissolution homogeneity, in the most backward system, add 2.8gNa 2sO 3, after reaction 100min, stopping heating and stirring, leave standstill and be cooled to room temperature, carry out suction filtration, collect filter residue, with pure water, filter residue being rinsed 2-3 all over being placed on 130 DEG C of freeze-day with constant temperature, ground 100-200 mesh sieve, then be placed in 50-60 DEG C of oven dry, collection sample.
Experiment detects:
(1) modified lignin of the lignin before modified and embodiment 1,2,3 of getting equivalent is scattered in water respectively, and phenomenon as shown in Figure 1.Lignin is before modified dispersed poor in water, easy reunion is side on the water, and modified lignin can be scattered in water uniformly, therefore in conjunction cream process, modified lignin can better be dispersed in lead plaster, is conducive to playing its effect in lead plaster process.
(2) in room temperature environment, test the modified lignin absorption PH=2 of above-mentioned lignin before modified and embodiment 1,2,3,3 the aqueous solution in Pb 2+, experimental result shows, compared with lignin before modified, under the environment of PH=2, in modified embodiment 1,2,3, lignin is to Pb 2+adsorbance improve 35.5%, 30.9%, 27.46% respectively; Under the environment of PH=3, adsorbance improves 82.67%, 77.84%, 63.40% respectively.
(3) Fig. 2 is the modified lignin absorption figure at different temperatures of lignin and embodiment 1,2,3 before modified.As seen from Figure 2, after the absorption of embodiment 1 ~ 3 modified lignin, in solution, Pb is remained 2+concentration significantly declines, and favors low temperature is in absorption, illustrates that modified lignin is to Pb 2+adsorptivity obviously strengthen, be applicable to doing heavy metal Pb in cathode additive agent and sewage in lead-acid battery field 2+process.

Claims (1)

1. a preparation method for high adsorption modified lignin, is characterized in that comprising the following steps:
(1) NaOH getting pure water quality 1-2% is dissolved in proportionaling alkali-forming solution in pure water;
(2) lignin getting pure water quality 3-5% adds in aqueous slkali, is stirred to lignin and dissolves completely;
(3) then step (2) solution is heated with stirring to 40 ~ 60 DEG C, gets H 2o 2slowly add, H 2o 2volume and lignin quality, than V:W=0.3 ~ 0.6, after in reaction 1-2min, are got 98% concentrated sulfuric acid and are slowly added, H 2sO 4volume and lignin quality, than V:W=0.25 ~ 0.4, continue stirring until solution and form homogeneous solution;
(4) Na that quality is lignin quality 40% ~ 70% is got 2sO 3, add in the mixed solution of step (3), and constantly stir, after sustained response 80 ~ 100min, stop heating and stir, leaving standstill cooling;
(5) after step (4) solution is cooled to room temperature, carry out suction filtration, collect filter residue, with pure water by filter residue washing and filtering, drying, grind, sieve, obtain high adsorption modified lignin.
CN201510356146.4A 2015-06-25 2015-06-25 High-adsorbability modified lignin preparation method Pending CN105186001A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105845941A (en) * 2016-05-20 2016-08-10 济南圣泉集团股份有限公司 Negative expander for lead-acid storage battery and application of negative expander in improvement of capacity performance of lead-acid storage battery
CN105968379A (en) * 2016-05-20 2016-09-28 济南圣泉集团股份有限公司 Lead-acid battery negative electrode expanding agent and application thereof in improving low-temperature properties of lead-acid battery
CN109659558A (en) * 2018-11-16 2019-04-19 佛山市科特电池有限公司 A kind of electric road vehicle lead storage battery green plate lead paste formula
CN110746613A (en) * 2019-10-25 2020-02-04 郑州大学 Functionalized ore source organic medicament and use method thereof
CN110791276A (en) * 2019-06-28 2020-02-14 大港油田集团有限责任公司 Stabilizer for polymer solution under high-temperature and high-salt conditions, and preparation method and application thereof
CN111224104A (en) * 2020-02-21 2020-06-02 超威电源集团有限公司 Carbon composite material, paste, battery and preparation method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104659369A (en) * 2015-03-26 2015-05-27 天能集团江苏科技有限公司 Preparation method of modified sodium lignosulfonate for lead-acid battery

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104659369A (en) * 2015-03-26 2015-05-27 天能集团江苏科技有限公司 Preparation method of modified sodium lignosulfonate for lead-acid battery

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105845941A (en) * 2016-05-20 2016-08-10 济南圣泉集团股份有限公司 Negative expander for lead-acid storage battery and application of negative expander in improvement of capacity performance of lead-acid storage battery
CN105968379A (en) * 2016-05-20 2016-09-28 济南圣泉集团股份有限公司 Lead-acid battery negative electrode expanding agent and application thereof in improving low-temperature properties of lead-acid battery
CN105845941B (en) * 2016-05-20 2019-06-04 济南圣泉集团股份有限公司 A kind of acid accumulator negative pole lead swelling agent and its application in improvement capacity of lead acid battery performance
CN105968379B (en) * 2016-05-20 2019-07-30 济南圣泉集团股份有限公司 A kind of acid accumulator negative pole lead swelling agent and its application in improvement lead-acid accumulator cryogenic property
CN109659558A (en) * 2018-11-16 2019-04-19 佛山市科特电池有限公司 A kind of electric road vehicle lead storage battery green plate lead paste formula
CN110791276A (en) * 2019-06-28 2020-02-14 大港油田集团有限责任公司 Stabilizer for polymer solution under high-temperature and high-salt conditions, and preparation method and application thereof
CN110791276B (en) * 2019-06-28 2021-09-07 大港油田集团有限责任公司 Stabilizer for polymer solution under high-temperature and high-salt conditions, and preparation method and application thereof
CN110746613A (en) * 2019-10-25 2020-02-04 郑州大学 Functionalized ore source organic medicament and use method thereof
CN111224104A (en) * 2020-02-21 2020-06-02 超威电源集团有限公司 Carbon composite material, paste, battery and preparation method

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Application publication date: 20151223