CN109231340A - A kind of preparation method of lightweight diatomite material for water treatment - Google Patents

A kind of preparation method of lightweight diatomite material for water treatment Download PDF

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Publication number
CN109231340A
CN109231340A CN201811227306.5A CN201811227306A CN109231340A CN 109231340 A CN109231340 A CN 109231340A CN 201811227306 A CN201811227306 A CN 201811227306A CN 109231340 A CN109231340 A CN 109231340A
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diatomite
water treatment
lightweight
preparation
mixture
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CN109231340B (en
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张文杰
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Inner Mongolia Heyuan Biotechnology Co ltd
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Shenyang Ligong University
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

Abstract

A kind of preparation method of lightweight diatomite material for water treatment, belongs to technical field of water treatment, including following processing steps: with hydrochloric acid solution to diatomite processing, obtaining activated diatomaceous earth;Activated diatomaceous earth is kept the temperature in the organic solvent containing zinc, obtains to surface and covers the diatomite of organic zinc;Then the activated diatomaceous earth of obtained coating organic zinc is mixed with iron salt solutions, through hydro-thermal reaction, drying, calcining, finally obtains lightweight diatomite material for water treatment.There is lighter density with lightweight diatomite material for water treatment prepared by this method, can quick adsorption organic pollutant, while there is the activity of decomposing organic pollutant under light illumination, have broad application prospects in water treatment field.

Description

A kind of preparation method of lightweight diatomite material for water treatment
Technical field
The invention belongs to technical field of water treatment, and in particular to a kind of preparation method of lightweight diatomite material for water treatment.
Background technique
With the aggravation of water pollution, the organic pollutant in water has to be purified using certain method, to reach The purpose of environment and human health is not endangered.Material for water treatment is essential one kind material in sewage purification process, usually Material for water treatment can by suction type by water organic pollutant remove.In order to reach better removal effect, need It is sufficiently mixed material for water treatment with water.Light material can more play a role, because with the comparable lightweight water process of water density Material is easy to be sufficiently mixed under mild agitation with water, promotes the diffusion and the rate of adsorption of pollutant.Lightweight diatomite is exactly Material a kind of in this way.
The biological silicalite that diatomite is made of the siliceous remains of diatom and other microorganisms have a large amount of, orderly The micropore of arrangement, to make diatomite that there is very big specific surface area, meanwhile, diatomite chemical stability is high, except being dissolved in hydrogen fluorine It is sour outer, any strong acid is not dissolved in, alkali is soluble in, it is without secondary pollution.Nevertheless, natural diatomaceous earth to the removal rate of phosphorus still not Be it is very high, cause mineral resources that cannot efficiently utilize, can not meet demand, therefore need to centainly be handled diatomite, make it Achieve the effect that preferably to remove water pollutant.
Summary of the invention
In view of the problems of the existing technology, the present invention is intended to provide a kind of preparation side of lightweight diatomite material for water treatment Method can be used for organic pollutant present in purified water;The water-purifying material can adsorb the organic matter in water and under light illumination It is allowed to degrade, is suitable for various water pollution field of purification.
A kind of preparation method of lightweight diatomite material for water treatment, including following preparation step.
(1) preparation of activated diatomaceous earth.
1. the 0.6mol/L hydrochloric acid solution of 500mL is mixed with 35g diatomite, 90 DEG C are heated the mixture to, it is warm herein Degree heat preservation 5h, then cools down, filters, rinsed with deionized water to filtrate pH=7, obtain solids A.
2., then in 800 DEG C of calcining 2h, being cooled to room temperature by solids A in 220 DEG C of dry 18h, activation diatom is obtained Soil.
(2) organic zinc is coated.
1. 5 ~ 10g ethylenediamine tetra-acetic acid, 8 ~ 11g zinc acetate, 3 ~ 6g emulsifier op-10 are added in 500mL dehydrated alcohol, Stirring forms solution A.
2. solution A and activated diatomaceous earth are mixed, 60 DEG C are heated the mixture to, keeps the temperature 120min at this temperature, is obtained To mixture A.
3. mixture A is evaporated to volume in 80 DEG C of water-baths no longer to reduce, mixture B is obtained.
(3) preparation of lightweight diatomite material for water treatment.
1. mixture B is mixed with the 0.08mol/L liquor ferri trichloridi of 300mL, stainless steel hydrothermal reaction kettle is moved into, 180 ~ 190 DEG C of reaction 30h, then cooling, filtering obtains solids B.
2., then in 650 ~ 780 DEG C of calcining 3h, being cooled to room temperature by solids B in 220 DEG C of dry 18h, obtaining lightweight Diatomite material for water treatment.
Wherein, 8 ~ 15mm of particle size of diatomite used, heap density 0.5g/cm3, specific surface area 60m2/ g, pore volume 0.75cm3/g。
The lightweight diatomite material for water treatment of preparation has following technical characteristic: the thickness of diatomite surface cladding ferrous acid zinc layers Degree is 0.9 ~ 1.2 μm, 120 ~ 170m of specific surface area2/ g, 0.6 ~ 0.8cm of pore volume3/ g, 0.6 ~ 0.7g/cm of heap density3
A kind of preparation method of lightweight diatomite material for water treatment of the invention has following excellent compared with prior art Point.
By the hydrochloric acid solution activation to diatomite, so that diatomite surface is with zinc ferrite active material layer with good Compatibility, ferrous acid zinc layers cladding is close not to block the original hole of diatomite again.Such lightweight diatomite material for water treatment has Lighter density is easy to mix with water, can give full play to the quick adsorption effect of material.Meanwhile zinc ferrite active material layer Activity with decomposing organic pollutant under light illumination, can absorption while decomposing pollutant, so as to use for a long time In the improvement of organic sewage.
Specific embodiment
Embodiment 1.
A kind of preparation method of lightweight diatomite material for water treatment, mainly includes the following steps that.
(1) preparation of activated diatomaceous earth.
1. the 0.6mol/L hydrochloric acid solution of 500mL is mixed with 35g diatomite, 90 DEG C are heated the mixture to, it is warm herein Degree heat preservation 5h, then cools down, filters, rinsed with deionized water to filtrate pH=7, obtain solids A.
2., then in 800 DEG C of calcining 2h, being cooled to room temperature by solids A in 220 DEG C of dry 18h, activation diatom is obtained Soil.
(2) organic zinc is coated.
1. 5g ethylenediamine tetra-acetic acid, 8g zinc acetate, 3g emulsifier op-10 are added in 500mL dehydrated alcohol, stirring is formed Solution A.
2. solution A and activated diatomaceous earth are mixed, 60 DEG C are heated the mixture to, keeps the temperature 120min at this temperature, is obtained To mixture A.
3. mixture A is evaporated to volume in 80 DEG C of water-baths no longer to reduce, mixture B is obtained.
(3) preparation of lightweight diatomite material for water treatment.
1. mixture B is mixed with the 0.08mol/L liquor ferri trichloridi of 300mL, stainless steel hydrothermal reaction kettle is moved into, 180 DEG C of reaction 30h, then cooling, filtering obtains solids B.
2., then in 650 DEG C of calcining 3h, being cooled to room temperature by solids B in 220 DEG C of dry 18h, obtaining lightweight diatom Native material for water treatment.
Wherein, the particle size 8mm of diatomite used, heap density 0.5g/cm3, specific surface area 60m2/ g, pore volume 0.75cm3/g。
The lightweight diatomite material for water treatment of preparation has following technical characteristic: the thickness of diatomite surface cladding ferrous acid zinc layers Degree is 0.9 μm, specific surface area 170m2/ g, pore volume 0.8cm3/ g, heap density 0.6g/cm3
Performance detection.
Preparing 200mL concentration is the azophloxine solution of 50 mg/L in beaker, is existed using visible spectrophotometer Its absorbance is measured at azophloxine maximum absorption wavelength 506nm.It weighs 100mg and passes through light silica prepared by embodiment 1 Diatomaceous earth material for water treatment is simultaneously added in azophloxine solution, and solution is moved to and stirs 20min in camera bellows.Take 5 mL solution mistakes Filter measures the absorbance of filtrate at wavelength 506nm.Resting solution is placed under 20 W ultraviolet germicidals and is irradiated, 30min is spaced Sampling and testing solution absorbance.Solution is azophloxine solution at lightweight diatomite water in the percent of decolourization of different time Manage the adsorption rate and photocatalytic activity on material.
It is learnt according to measurement result, after 20min is protected from light adsorption process, azophloxine is at lightweight diatomite water Reach adsorption-desorption balance on reason material, saturation balance adsorption rate is 3.2%.Through ultraviolet-sterilization light irradiation, azophloxine Photocatalytic degradation reaction occurs;After 120min reacts, azophloxine solution decolourizes completely, and percent of decolourization reaches 100%.
Embodiment 2.
A kind of preparation method of lightweight diatomite material for water treatment, mainly includes the following steps that.
(1) preparation of activated diatomaceous earth.
1. the 0.6mol/L hydrochloric acid solution of 500mL is mixed with 35g diatomite, 90 DEG C are heated the mixture to, it is warm herein Degree heat preservation 5h, then cools down, filters, rinsed with deionized water to filtrate pH=7, obtain solids A.
2., then in 800 DEG C of calcining 2h, being cooled to room temperature by solids A in 220 DEG C of dry 18h, activation diatom is obtained Soil.
(2) organic zinc is coated.
1. 7g ethylenediamine tetra-acetic acid, 9g zinc acetate, 4g emulsifier op-10 are added in 500mL dehydrated alcohol, stirring is formed Solution A.
2. solution A and activated diatomaceous earth are mixed, 60 DEG C are heated the mixture to, keeps the temperature 120min at this temperature, is obtained To mixture A.
3. mixture A is evaporated to volume in 80 DEG C of water-baths no longer to reduce, mixture B is obtained.
(3) preparation of lightweight diatomite material for water treatment.
1. mixture B is mixed with the 0.08mol/L liquor ferri trichloridi of 300mL, stainless steel hydrothermal reaction kettle is moved into, 185 DEG C of reaction 30h, then cooling, filtering obtains solids B.
2., then in 710 DEG C of calcining 3h, being cooled to room temperature by solids B in 220 DEG C of dry 18h, obtaining lightweight diatom Native material for water treatment.
The particle size 11mm of diatomite used, heap density 0.5g/cm3, specific surface area 60m2/ g, pore volume 0.75cm3/ g。
The lightweight diatomite material for water treatment of preparation has following technical characteristic: the thickness of diatomite surface cladding ferrous acid zinc layers Degree is 1.0 μm, specific surface area 140m2/ g, pore volume 0.7cm3/ g, heap density 0.63g/cm3
Embodiment 3.
A kind of preparation method of lightweight diatomite material for water treatment, mainly includes the following steps that.
(1) preparation of activated diatomaceous earth.
1. the 0.6mol/L hydrochloric acid solution of 500mL is mixed with 35g diatomite, 90 DEG C are heated the mixture to, it is warm herein Degree heat preservation 5h, then cools down, filters, rinsed with deionized water to filtrate pH=7, obtain solids A.
2., then in 800 DEG C of calcining 2h, being cooled to room temperature by solids A in 220 DEG C of dry 18h, activation diatom is obtained Soil.
(2) organic zinc is coated.
1. 10g ethylenediamine tetra-acetic acid, 11g zinc acetate, 6g emulsifier op-10 are added in 500mL dehydrated alcohol, shape is stirred At solution A.
2. solution A and activated diatomaceous earth are mixed, 60 DEG C are heated the mixture to, keeps the temperature 120min at this temperature, is obtained To mixture A.
3. mixture A is evaporated to volume in 80 DEG C of water-baths no longer to reduce, mixture B is obtained.
(3) preparation of lightweight diatomite material for water treatment.
1. mixture B is mixed with the 0.08mol/L liquor ferri trichloridi of 300mL, stainless steel hydrothermal reaction kettle is moved into, 190 DEG C of reaction 30h, then cooling, filtering obtains solids B.
2., then in 780 DEG C of calcining 3h, being cooled to room temperature by solids B in 220 DEG C of dry 18h, obtaining lightweight diatom Native material for water treatment.
The particle size 15mm of diatomite used, heap density 0.5g/cm3, specific surface area 60m2/ g, pore volume 0.75cm3/ g。
The lightweight diatomite material for water treatment of preparation has following technical characteristic: the thickness of diatomite surface cladding ferrous acid zinc layers Degree is 1.2 μm, specific surface area 120m2/ g, pore volume 0.6cm3/ g, heap density 0.7g/cm3
Comparative experiments.
1 ordinary silicon diatomaceous earth of comparative example.
Each 100mg of ordinary silicon diatomaceous earth of lightweight diatomite material for water treatment and comparative example 1 made from Example 1 respectively, It is added in the azophloxine solution that 200mL concentration is 50 mg/L, there are 2 groups of samples, azo fluorescence is removed to every group of sample Pink efficiency is compared, and with embodiment 1, testing result see the table below method for testing performance.

Claims (3)

1. a kind of preparation method of lightweight diatomite material for water treatment, which is characterized in that the preparation method includes following technique steps It is rapid:
(1) preparation of activated diatomaceous earth
1. the 0.6mol/L hydrochloric acid solution of 500mL is mixed with 35g diatomite, 90 DEG C are heated the mixture to, is protected in this temperature Warm 5h, then cools down, and filtering is rinsed to filtrate pH=7 with deionized water, obtains solids A;
2., then in 800 DEG C of calcining 2h, being cooled to room temperature by solids A in 220 DEG C of dry 18h, obtaining activated diatomaceous earth;
(2) organic zinc is coated
1. 5 ~ 10g ethylenediamine tetra-acetic acid, 8 ~ 11g zinc acetate, 3 ~ 6g emulsifier op-10 are added in 500mL dehydrated alcohol, stirring Form solution A;
2. solution A and activated diatomaceous earth are mixed, 60 DEG C are heated the mixture to, keeps the temperature 120min at this temperature, is mixed Close object A;
3. mixture A is evaporated to volume in 80 DEG C of water-baths no longer to reduce, mixture B is obtained;
(3) preparation of lightweight diatomite material for water treatment
1. mixture B is mixed with the 0.08mol/L liquor ferri trichloridi of 300mL, stainless steel hydrothermal reaction kettle is moved into, 180 ~ 190 DEG C of reaction 30h, then cooling, filtering obtains solids B;
2., then in 650 ~ 780 DEG C of calcining 3h, being cooled to room temperature by solids B in 220 DEG C of dry 18h, obtaining lightweight diatom Native material for water treatment.
2. a kind of lightweight diatomite material for water treatment according to claim 1, which is characterized in that the particle of the diatomite 8 ~ 15mm of size, heap density 0.5g/cm3, specific surface area 60m2/ g, pore volume 0.75cm3/g。
3. a kind of lightweight diatomite material for water treatment according to claim 1, which is characterized in that prepared lightweight diatom Native material for water treatment, in diatomite surface coated ferrous acid zinc layers with a thickness of 0.9 ~ 1.2 μm, 120 ~ 170m of specific surface area2/ g, 0.6 ~ 0.8cm of pore volume3/ g, 0.6 ~ 0.7g/cm of heap density3
CN201811227306.5A 2018-10-22 2018-10-22 Preparation method of light diatomite water treatment material Active CN109231340B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114146681A (en) * 2021-11-30 2022-03-08 广州东联环保科技有限公司 Composite material for treating nitrogen-containing sewage and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139195A (en) * 2011-01-07 2011-08-03 中国林业科学研究院林产化学工业研究所 Gas-liquid double-phase reactor and application thereof in production of fatty acid methyl ester in presence of solid-acid catalyst
CN103194222A (en) * 2013-04-18 2013-07-10 扬州大学 Preparation method and application of Fe3O4/ZnO composite nano-particles
CN103754953A (en) * 2014-01-28 2014-04-30 南京信息工程大学 Preparation method of multi-morphologynano-sized zinc ferrite
US20160102001A1 (en) * 2014-10-09 2016-04-14 National Tsing Hua University Kit for wastewater treatment, and manufacturing method for and use of photocatalyst

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139195A (en) * 2011-01-07 2011-08-03 中国林业科学研究院林产化学工业研究所 Gas-liquid double-phase reactor and application thereof in production of fatty acid methyl ester in presence of solid-acid catalyst
CN103194222A (en) * 2013-04-18 2013-07-10 扬州大学 Preparation method and application of Fe3O4/ZnO composite nano-particles
CN103754953A (en) * 2014-01-28 2014-04-30 南京信息工程大学 Preparation method of multi-morphologynano-sized zinc ferrite
US20160102001A1 (en) * 2014-10-09 2016-04-14 National Tsing Hua University Kit for wastewater treatment, and manufacturing method for and use of photocatalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114146681A (en) * 2021-11-30 2022-03-08 广州东联环保科技有限公司 Composite material for treating nitrogen-containing sewage and preparation method and application thereof

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