CN105435752A - Heavy metal ions absorbent and preparation method thereof - Google Patents

Heavy metal ions absorbent and preparation method thereof Download PDF

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Publication number
CN105435752A
CN105435752A CN201610004623.5A CN201610004623A CN105435752A CN 105435752 A CN105435752 A CN 105435752A CN 201610004623 A CN201610004623 A CN 201610004623A CN 105435752 A CN105435752 A CN 105435752A
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heavy metal
parts
pine bark
absorbent
metal ions
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CN201610004623.5A
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郭菲
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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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024—Compounds of Zn, Cd, Hg
    • B01J20/0244—Compounds of Zn
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0262—Compounds of O, S, Se, Te
    • B01J20/0266—Compounds of S
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • 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
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention relates to a heavy metal ions absorbent and a preparation method thereof. The heavy metal ions absorbent is prepared from the following raw materials in parts by weight: 200 to 300 parts of pine bark, 4 to 8 parts of zinc sulfide, 5 to 7 parts of iron sulfide, 10 to 20 parts of (3-mercaptopropyl) trimethoxysilane, 50 to 60 parts of kieselguhr, 20 to 40 parts of ethylene glycol, 10 to 20 parts of hydrochloric acid, 10 to 14 parts of hexadecyl trimethyl ammonium bromide and 400 to 500 parts of deionized water. The heavy metal ions absorbent and the preparation method disclosed by the invention have the advantages that the pine bark is well-sourced and relatively low in cost; a molecular sieve carrier is adopted to carry out ion exchange without secondary pollution; the heavy metal ions absorbent has a favorable removal effect on liquid-phase heavy metal and heavy metal ions.

Description

A kind of heavy metal absorbent and preparation method thereof
Technical field
The present invention relates to environmental technology field, particularly relate to a kind of heavy metal absorbent and preparation method thereof.
Background technology
In the fast development process of China's economy and industrial technology, the environmental problem brought more and more comes into one's own, and sewage treating material has become the important component part in sewage disposal technology, receives the concern of every field equally; And lack for the kind of sewage disposal at present, greatly limit the selection of sewage treating material, therefore, develop that a kind of to be applicable to having heavy metal ions in wastewater adsorption efficiency of sewage disposal good, adsorbance is large, the sorbing material of excellent in mechanical performance, to enriching sewage treating material, promotes that the development of sewage disposal is significant.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of heavy metal absorbent and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of heavy metal absorbent, is made up of the raw material of following weight portion: pine bark 200-300, zinc sulphide 4-8, iron sulfide 5-7, trimethoxy sulfydryl acrylsilanes 10-20, diatomite 50-60, ethylene glycol 20-40, hydrochloric acid 10-20, softex kw 10-14, deionized water 400-500.
Optimize, a kind of heavy metal absorbent, is made up of the raw material of following weight portion: pine bark 250, zinc sulphide 6, iron sulfide 6, trimethoxy sulfydryl acrylsilanes 15, diatomite 55, ethylene glycol 30, hydrochloric acid 15, softex kw 12, deionized water 450.
The preparation method of described heavy metal absorbent, comprises the following steps:
Step 1: pine bark is inserted in smelting furnace and carbonizes, carburizing temperature 800-1000 DEG C, carbonization time 20-30min;
Step 2: pass into oxygen content in nitrogen to smelting furnace and be less than 400ppm in smelting furnace, it is for subsequent use to be down to room temperature;
Step 3: the pine bark after charing step 2 obtained grinds, 600 orders sieve;
Step 4: carry out steam activation to the charing powder that step 3 obtains, evenly by the carbon dioxide 20min containing 5% carbon monoxide in charing powder;
Step 5: grind after diatomite drying, 600 orders sieve, and activate pine bark and carbonize powder and mix, stir for subsequent use after sieving with step 4 gained;
Step 6: iron sulfide and zinc sulphide are added in deionized water, magnetic agitation 30min;
Step 7: mixture step 5 obtained adds in the mixed solution that step 6 obtains, and filter after sonic oscillation 30min, filtrate is drying for standby at room temperature;
Step 8: add trimethoxy sulfydryl acrylsilanes in ethylene glycol, stir and add hydrochloric acid, ultrasonic process 20min;
Step 9: mixed liquor step 8 obtained adds softex kw, stir while add the dry thing of step 7 gained, magnetic agitation 30min, heating water bath condensing reflux 5-6h at 80 DEG C, after reactant is down to room temperature, solid vacuum drying 24h at 20 DEG C is isolated in washing, both obtains heavy metal absorbent.
Advantage of the present invention is: pine bark wide material sources of the present invention, and cost is lower, and adopt molecular sieve carrier to carry out ion-exchange, can not cause secondary pollution, the present invention has good removal effect for the heavy metal of liquid phase and heavy metal ion.
Detailed description of the invention
Embodiment 1:
A kind of heavy metal absorbent, is made up of the raw material of following weight portion: pine bark 200, zinc sulphide 4, iron sulfide 5, trimethoxy sulfydryl acrylsilanes 10, diatomite 50, ethylene glycol 20, hydrochloric acid 10, softex kw 10, deionized water 400.
The preparation method of described heavy metal absorbent, comprises the following steps:
Step 1: pine bark is inserted in smelting furnace and carbonizes, carburizing temperature 800-1000 DEG C, carbonization time 20-30min;
Step 2: pass into oxygen content in nitrogen to smelting furnace and be less than 400ppm in smelting furnace, it is for subsequent use to be down to room temperature;
Step 3: the pine bark after charing step 2 obtained grinds, 600 orders sieve;
Step 4: carry out steam activation to the charing powder that step 3 obtains, evenly by the carbon dioxide 20min containing 5% carbon monoxide in charing powder;
Step 5: grind after diatomite drying, 600 orders sieve, and activate pine bark and carbonize powder and mix, stir for subsequent use after sieving with step 4 gained;
Step 6: iron sulfide and zinc sulphide are added in deionized water, magnetic agitation 30min;
Step 7: mixture step 5 obtained adds in the mixed solution that step 6 obtains, and filter after sonic oscillation 30min, filtrate is drying for standby at room temperature;
Step 8: add trimethoxy sulfydryl acrylsilanes in ethylene glycol, stir and add hydrochloric acid, ultrasonic process 20min;
Step 9: mixed liquor step 8 obtained adds softex kw, stir while add the dry thing of step 7 gained, magnetic agitation 30min, heating water bath condensing reflux 5-6h at 80 DEG C, after reactant is down to room temperature, solid vacuum drying 24h at 20 DEG C is isolated in washing, both obtains heavy metal absorbent.
Embodiment 2:
A kind of heavy metal absorbent, is made up of the raw material of following weight portion: pine bark 300, zinc sulphide 8, iron sulfide 7, trimethoxy sulfydryl acrylsilanes 20, diatomite 60, ethylene glycol 40, hydrochloric acid 20, softex kw 14, deionized water 500.
The preparation method of described heavy metal absorbent, comprises the following steps:
Step 1: pine bark is inserted in smelting furnace and carbonizes, carburizing temperature 800-1000 DEG C, carbonization time 20-30min;
Step 2: pass into oxygen content in nitrogen to smelting furnace and be less than 400ppm in smelting furnace, it is for subsequent use to be down to room temperature;
Step 3: the pine bark after charing step 2 obtained grinds, 600 orders sieve;
Step 4: carry out steam activation to the charing powder that step 3 obtains, evenly by the carbon dioxide 20min containing 5% carbon monoxide in charing powder;
Step 5: grind after diatomite drying, 600 orders sieve, and activate pine bark and carbonize powder and mix, stir for subsequent use after sieving with step 4 gained;
Step 6: iron sulfide and zinc sulphide are added in deionized water, magnetic agitation 30min;
Step 7: mixture step 5 obtained adds in the mixed solution that step 6 obtains, and filter after sonic oscillation 30min, filtrate is drying for standby at room temperature;
Step 8: add trimethoxy sulfydryl acrylsilanes in ethylene glycol, stir and add hydrochloric acid, ultrasonic process 20min;
Step 9: mixed liquor step 8 obtained adds softex kw, stir while add the dry thing of step 7 gained, magnetic agitation 30min, heating water bath condensing reflux 5-6h at 80 DEG C, after reactant is down to room temperature, solid vacuum drying 24h at 20 DEG C is isolated in washing, both obtains heavy metal absorbent.
Embodiment 3:
A kind of heavy metal absorbent, is made up of the raw material of following weight portion: pine bark 250, zinc sulphide 6, iron sulfide 6, trimethoxy sulfydryl acrylsilanes 15, diatomite 55, ethylene glycol 30, hydrochloric acid 15, softex kw 12, deionized water 450.
The preparation method of described heavy metal absorbent, comprises the following steps:
Step 1: pine bark is inserted in smelting furnace and carbonizes, carburizing temperature 800-1000 DEG C, carbonization time 20-30min;
Step 2: pass into oxygen content in nitrogen to smelting furnace and be less than 400ppm in smelting furnace, it is for subsequent use to be down to room temperature;
Step 3: the pine bark after charing step 2 obtained grinds, 600 orders sieve;
Step 4: carry out steam activation to the charing powder that step 3 obtains, evenly by the carbon dioxide 20min containing 5% carbon monoxide in charing powder;
Step 5: grind after diatomite drying, 600 orders sieve, and activate pine bark and carbonize powder and mix, stir for subsequent use after sieving with step 4 gained;
Step 6: iron sulfide and zinc sulphide are added in deionized water, magnetic agitation 30min;
Step 7: mixture step 5 obtained adds in the mixed solution that step 6 obtains, and filter after sonic oscillation 30min, filtrate is drying for standby at room temperature;
Step 8: add trimethoxy sulfydryl acrylsilanes in ethylene glycol, stir and add hydrochloric acid, ultrasonic process 20min;
Step 9: mixed liquor step 8 obtained adds softex kw, stir while add the dry thing of step 7 gained, magnetic agitation 30min, heating water bath condensing reflux 5-6h at 80 DEG C, after reactant is down to room temperature, solid vacuum drying 24h at 20 DEG C is isolated in washing, both obtains heavy metal absorbent.
Detection is carried out to embodiment 1-3 gained heavy metal absorbent and obtains following table:
Table 1 embodiment 1-3 Performance Detection table;
Mercury clearance (%) Removal of heavy metal ions rate (%) Organic benzene, organic refuse clearance (%)
Embodiment 1 92 89 84
Embodiment 2 95 91 85
Embodiment 3 97 94 87
Can see that heavy metal of the present invention has good adsorption effect by table 1, also have certain adsorption effect for debirs.

Claims (3)

1. a heavy metal absorbent, is characterized in that: be made up of the raw material of following weight portion: pine bark 200-300, zinc sulphide 4-8, iron sulfide 5-7, trimethoxy sulfydryl acrylsilanes 10-20, diatomite 50-60, ethylene glycol 20-40, hydrochloric acid 10-20, softex kw 10-14, deionized water 400-500.
2. a heavy metal absorbent as claimed in claim 1, is characterized in that: be made up of the raw material of following weight portion: pine bark 250, zinc sulphide 6, iron sulfide 6, trimethoxy sulfydryl acrylsilanes 15, diatomite 55, ethylene glycol 30, hydrochloric acid 15, softex kw 12, deionized water 450.
3. a preparation method for heavy metal absorbent as claimed in claim 1 or 2, is characterized in that comprising the following steps:
Step 1: pine bark is inserted in smelting furnace and carbonizes, carburizing temperature 800-1000 DEG C, carbonization time 20-30min;
Step 2: pass into oxygen content in nitrogen to smelting furnace and be less than 400ppm in smelting furnace, it is for subsequent use to be down to room temperature;
Step 3: the pine bark after charing step 2 obtained grinds, 600 orders sieve;
Step 4: carry out steam activation to the charing powder that step 3 obtains, evenly by the carbon dioxide 20min containing 5% carbon monoxide in charing powder;
Step 5: grind after diatomite drying, 600 orders sieve, and activate pine bark and carbonize powder and mix, stir for subsequent use after sieving with step 4 gained;
Step 6: iron sulfide and zinc sulphide are added in deionized water, magnetic agitation 30min;
Step 7: mixture step 5 obtained adds in the mixed solution that step 6 obtains, and filter after sonic oscillation 30min, filtrate is drying for standby at room temperature;
Step 8: add trimethoxy sulfydryl acrylsilanes in ethylene glycol, stir and add hydrochloric acid, ultrasonic process 20min;
Step 9: mixed liquor step 8 obtained adds softex kw, stir while add the dry thing of step 7 gained, magnetic agitation 30min, heating water bath condensing reflux 5-6h at 80 DEG C, after reactant is down to room temperature, solid vacuum drying 24h at 20 DEG C is isolated in washing, both obtains heavy metal absorbent.
CN201610004623.5A 2016-01-05 2016-01-05 Heavy metal ions absorbent and preparation method thereof Withdrawn CN105435752A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105854417A (en) * 2016-05-12 2016-08-17 浙江国科生态技术研究有限公司 Active filter medium
CN106390936A (en) * 2016-12-07 2017-02-15 郑州源冉生物技术有限公司 Illite adsorbent as well as preparation method and application thereof
CN106423046A (en) * 2016-12-07 2017-02-22 郑州源冉生物技术有限公司 Diatomite adsorbent as well as preparation method and application of diatomite adsorbent
CN106517664A (en) * 2016-12-07 2017-03-22 广西南宁科茂企业信息咨询有限公司 Pig farm sewage treatment method
CN107384414A (en) * 2017-06-28 2017-11-24 防城港市水利水电勘测设计院 Rice field heavy metal absorbent
CN107537448A (en) * 2017-10-17 2018-01-05 诸暨马谷亲科技有限公司 Medicament of heavy metal and preparation method thereof in a kind of removal trade effluent
CN111408339A (en) * 2020-05-09 2020-07-14 中国科学院生态环境研究中心 Preparation method and application of sepiolite composite adsorbent loaded with nano zinc sulfide

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105854417A (en) * 2016-05-12 2016-08-17 浙江国科生态技术研究有限公司 Active filter medium
CN106390936A (en) * 2016-12-07 2017-02-15 郑州源冉生物技术有限公司 Illite adsorbent as well as preparation method and application thereof
CN106423046A (en) * 2016-12-07 2017-02-22 郑州源冉生物技术有限公司 Diatomite adsorbent as well as preparation method and application of diatomite adsorbent
CN106517664A (en) * 2016-12-07 2017-03-22 广西南宁科茂企业信息咨询有限公司 Pig farm sewage treatment method
CN107384414A (en) * 2017-06-28 2017-11-24 防城港市水利水电勘测设计院 Rice field heavy metal absorbent
CN107537448A (en) * 2017-10-17 2018-01-05 诸暨马谷亲科技有限公司 Medicament of heavy metal and preparation method thereof in a kind of removal trade effluent
CN111408339A (en) * 2020-05-09 2020-07-14 中国科学院生态环境研究中心 Preparation method and application of sepiolite composite adsorbent loaded with nano zinc sulfide

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Application publication date: 20160330