CN106693900A - Zeolite-based heavy metal adsorption material and preparation method thereof - Google Patents

Zeolite-based heavy metal adsorption material and preparation method thereof Download PDF

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Publication number
CN106693900A
CN106693900A CN201611123800.8A CN201611123800A CN106693900A CN 106693900 A CN106693900 A CN 106693900A CN 201611123800 A CN201611123800 A CN 201611123800A CN 106693900 A CN106693900 A CN 106693900A
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parts
zeolite
mixture
adsorption material
sodium
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沈美珍
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YUYAO QINGDA MACHINERY Co Ltd
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YUYAO QINGDA MACHINERY Co Ltd
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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
    • B01J20/22—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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
    • 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
    • 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
    • B01J20/16—Alumino-silicates
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • 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
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents

Abstract

The invention discloses a zeolite-based heavy metal adsorption material which consists of the following raw materials in parts by weight: 42-50 parts of zeolite, 10-15 parts of sodium silicate, 3-7 parts of butyl stearate, 2-5 parts of tetrabutyl titanate, 1-3 parts of magnesium sulfate and 4-7 parts of sodium diethylene triamine pentacetate. The invention further discloses a preparation method of the zeolite-based heavy metal adsorption material. The zeolite-based heavy metal adsorption material disclosed by the invention is good in adsorption effect, convenient to use, widely applicable to treatment on various types of heavy metal sewage, low in use cost and beneficial to increase of economic benefits of sewage treatment enterprises, and the adsorption effect of the zeolite-based heavy metal adsorption material is prior to that of common zeolite.

Description

A kind of heavy-metal adsorption material based on zeolite and preparation method thereof
Technical field
The present invention relates to heavy metal processing technology field, specifically a kind of heavy-metal adsorption material and its system based on zeolite Preparation Method.
Background technology
Science and technology is a double-edged sword, and scientific and technical fast development, promotes expanding economy since 21 century, improves people The living standard of the people, however, at the same time, the mankind have also paid the cost of heaviness.Due to Industrial " three Waste " motor-vehicle tail-gas The use of discharge, sewage irrigation and agricultural chemicals, herbicide, chemical fertilizer etc. and the development of mining industry, seriously pollute soil, water quality and Air.
Heavy metal pollution is a kind of pollution great to human health damage.At present for heavy metal containing sewage, mainly pass through Chemical method, physisorphtion and bioanalysis are processed, and wherein physisorphtion is because easy to use, and processing cost is low, using compared with For extensive.
Zeolite is a kind of brand-new material, is widely used in the departments such as industry, agricultural, national defence, and its purposes also exists Constantly open up.Zeolite is used as ion-exchanger, adsorption separating agent, drier, catalyst, cement additive.Oil, In chemical industry, chemical isomerization, reformation, alkylation, the discrimination of catalytic cracking, hydrocracking and oil as petroleum refining Change；Air-liquid purification, separation and storage agent；Water softening, seawater desalination.It is conventional in heavy metal physical absorption process field The adsorption effect of zeolite heavy metal is unsatisfactory, if can be compounded by the modified and raw material to zeolite, makes one kind and is based on The sorbing material of zeolite, improves the adsorption effect of its heavy metal, undoubtedly by with important market value.
The content of the invention
It is an object of the invention to provide a kind of heavy-metal adsorption material based on zeolite and preparation method thereof, with solution State the problem proposed in background technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：Zeolite 42-50 parts, silicon Sour sodium 10-15 parts, butyl stearate 3-7 parts, tetrabutyl titanate 2-5 parts, magnesium sulfate 1-3 parts, the sodium of diethylene triamine pentacetic acid (DTPA) five 4-7 parts.
As further scheme of the invention：It is made up of the following raw material according to weight：Zeolite 43-49 parts, sodium metasilicate 12- 14 parts, butyl stearate 4-6 parts, tetrabutyl titanate 3-4 parts, magnesium sulfate 1.3-2.7 parts, the sodium 5-6 of diethylene triamine pentacetic acid (DTPA) five Part.
As further scheme of the invention：It is made up of the following raw material according to weight：46 parts of zeolite, sodium metasilicate 13 Part, 5 parts of butyl stearate, 3 parts of tetrabutyl titanate, 1.9 parts of magnesium sulfate, 5 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
The preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 300-400 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds the 5-8 times of deionized water of weight, after stirring mixing 3-5h, stand 2h, Supernatant liquor and lower sediment are discarded, zeolite suspension is obtained；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, Mixing 2-3h is stirred at 60-70 DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 5-10% is slowly added dropwise in the first mixture, salpeter solution is in 30-40min drops Add it is complete, and during dropwise addition stir, after completion of dropping, obtain the second mixture；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 50-60min, obtains the 3rd mixture, surpassed Acoustic wave temperature is 70-80 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 200-300 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2- 3h, obtains powder, by granulation for powders.
As further scheme of the invention：Step 4) in, the concentration of the salpeter solution is 3-4mol/L.
Compared with prior art, the beneficial effects of the invention are as follows：
The advantages of good adsorption effect of sorbing material heavy metal ion prepared by the present invention, its adsorption effect is better than conventional boiling Stone.Sorbing material prepared by the present invention is easy to use, can be widely applied for the treatment of various heavy metal containing sewages, and use cost It is low, be conducive to improving the economic benefit of sewage disposal enterprise.
Specific embodiment
Technical scheme is described in more detail with reference to specific embodiment.
Embodiment 1
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：42 parts of zeolite, sodium metasilicate 10 parts, 3 parts of butyl stearate, 2 parts of tetrabutyl titanate, 1 part of magnesium sulfate, 4 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
In the present embodiment, the preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 300 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds 5 times of deionized waters of weight, after stirring mixing 3h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, 60 Mixing 2h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 5% is slowly added dropwise in the first mixture, salpeter solution is dripped in 30min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture, wherein, the concentration of the salpeter solution is 3mol/L；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 50min, obtains the 3rd mixture, ultrasound Ripple temperature is 70 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 200 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2h, obtains powder, by granulation for powders.
Embodiment 2
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：43 parts of zeolite, sodium metasilicate 12 parts, 6 parts of butyl stearate, 4 parts of tetrabutyl titanate, 1.3 parts of magnesium sulfate, 6 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
In the present embodiment, the preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 350 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds 6 times of deionized waters of weight, after stirring mixing 3h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, 65 Mixing 2h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 6% is slowly added dropwise in the first mixture, salpeter solution is dripped in 35min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture, wherein, the concentration of the salpeter solution is 3mol/L；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 55min, obtains the 3rd mixture, ultrasound Ripple temperature is 80 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 200 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2.5h, obtains powder, by granulation for powders.
Embodiment 3
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：46 parts of zeolite, sodium metasilicate 13 parts, 5 parts of butyl stearate, 3 parts of tetrabutyl titanate, 1.9 parts of magnesium sulfate, 5 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
In the present embodiment, the preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 400 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds 7 times of deionized waters of weight, after stirring mixing 4h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, 65 Mixing 2.5h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 8% is slowly added dropwise in the first mixture, salpeter solution is dripped in 35min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture, wherein, the concentration of the salpeter solution is 3.5mol/L；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 55min, obtains the 3rd mixture, ultrasound Ripple temperature is 75 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 300 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2.5h, obtains powder, by granulation for powders.
Embodiment 4
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：49 parts of zeolite, sodium metasilicate 14 parts, 4 parts of butyl stearate, 3 parts of tetrabutyl titanate, 2.7 parts of magnesium sulfate, 5 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
In the present embodiment, the preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 400 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds 7 times of deionized waters of weight, after stirring mixing 4h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, 67 Mixing 2.5h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 8% is slowly added dropwise in the first mixture, salpeter solution is dripped in 35min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture, wherein, the concentration of the salpeter solution is 3.5mol/L；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 56min, obtains the 3rd mixture, ultrasound Ripple temperature is 78 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 200 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2h, obtains powder, by granulation for powders.
Embodiment 5
A kind of heavy-metal adsorption material based on zeolite, is made up of the following raw material according to weight：50 parts of zeolite, sodium metasilicate 15 parts, 7 parts of butyl stearate, 5 parts of tetrabutyl titanate, 3 parts of magnesium sulfate, 7 parts of five sodium of diethylene triamine pentacetic acid (DTPA).
In the present embodiment, the preparation method of the heavy-metal adsorption material based on zeolite, step is as follows：
1) zeolite is weighed, after ultramicro grinding, 400 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds 8 times of deionized waters of weight, after stirring mixing 5h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, 70 Mixing 3h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 10% is slowly added dropwise in the first mixture, salpeter solution is dripped in 40min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture, wherein, the concentration of the salpeter solution is 4mol/L；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 60min, obtains the 3rd mixture, ultrasound Ripple temperature is 80 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 300 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 3h, obtains powder, by granulation for powders.
The advantages of good adsorption effect of sorbing material heavy metal ion prepared by the present invention, its adsorption effect is better than conventional boiling Stone.Sorbing material prepared by the present invention is easy to use, can be widely applied for the treatment of various heavy metal containing sewages, and use cost It is low, be conducive to improving the economic benefit of sewage disposal enterprise.
Better embodiment of the invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party Formula, in the ken that one skilled in the relevant art possesses, can also be on the premise of present inventive concept not be departed from Various changes can be made.

Claims (5)

1. a kind of heavy-metal adsorption material based on zeolite, it is characterised in that be made up of the following raw material according to weight：Zeolite 42-50 parts, sodium metasilicate 10-15 parts, butyl stearate 3-7 parts, tetrabutyl titanate 2-5 parts, magnesium sulfate 1-3 parts, diethylenetriamine Sodium 4-7 parts of pentaacetic acid five.
2. the heavy-metal adsorption material based on zeolite according to claim 1, it is characterised in that by following according to weight Raw material is constituted：Zeolite 43-49 parts, sodium metasilicate 12-14 parts, butyl stearate 4-6 parts, tetrabutyl titanate 3-4 parts, magnesium sulfate 1.3- 2.7 parts, sodium 5-6 parts of diethylene triamine pentacetic acid (DTPA) five.
3. the heavy-metal adsorption material based on zeolite according to claim 2, it is characterised in that by following according to weight Raw material is constituted：46 parts of zeolite, 13 parts of sodium metasilicate, 5 parts of butyl stearate, 3 parts of tetrabutyl titanate, 1.9 parts of magnesium sulfate, divinyl three 5 parts of five sodium of triamine pentaacetic acid.
4. a kind of preparation method of heavy-metal adsorption material based on zeolite as described in claim 1-3 is any, its feature exists In step is as follows：
1) zeolite is weighed, after ultramicro grinding, 300-400 mesh sieves is crossed, zeolite micro mist is obtained；
2) zeolite micro mist is placed in container, adds the 5-8 times of deionized water of weight, after stirring mixing 3-5h, stand 2h, discarded Supernatant liquor and lower sediment, obtain zeolite suspension；
3) sodium metasilicate, tetrabutyl titanate and the sodium of diethylene triamine pentacetic acid (DTPA) five are weighed, is added into zeolite suspension, in 60-70 Mixing 2-3h is stirred at DEG C, the first mixture is obtained；
4) to the salpeter solution that its gross weight 5-10% is slowly added dropwise in the first mixture, salpeter solution is dripped in 30-40min Finish, and stirred during dropwise addition, after completion of dropping, obtain the second mixture；
5) the second mixture is put into processor for ultrasonic wave, ultrasonication 50-60min, obtains the 3rd mixture, ultrasonic wave Temperature is 70-80 DEG C, and ultrasonic power is 1000W；
6) the 3rd mixture is dried in an oven, is ground, cross 200-300 mesh sieves, obtain the 4th mixture；
7) butyl stearate and magnesium sulfate are weighed, is added into the 4th mixture, after being uniformly mixed, ball milling mixing 2-3h, Powder is obtained, by granulation for powders.
5. the preparation method of the heavy-metal adsorption material based on zeolite according to claim 4, it is characterised in that step 4) In, the concentration of the salpeter solution is 3-4mol/L.
CN201611123800.8A 2016-12-08 2016-12-08 Zeolite-based heavy metal adsorption material and preparation method thereof Pending CN106693900A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080047902A1 (en) * 2006-08-28 2008-02-28 Basf Catalysts Llc Media for the removal of heavy metals and volatile byproducts from drinking water
CN101148273A (en) * 2006-09-20 2008-03-26 张金香 Sewage processing agent and its preparation method
CN103641226A (en) * 2013-12-26 2014-03-19 张�成 Heavy metal sewage treating agent and preparation method thereof
JP2015231610A (en) * 2014-06-10 2015-12-24 国立大学法人山口大学 Method for processing contaminated water
CN105344318A (en) * 2015-10-30 2016-02-24 王立鑫 Active carbon composite material for water purification, and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080047902A1 (en) * 2006-08-28 2008-02-28 Basf Catalysts Llc Media for the removal of heavy metals and volatile byproducts from drinking water
CN101148273A (en) * 2006-09-20 2008-03-26 张金香 Sewage processing agent and its preparation method
CN103641226A (en) * 2013-12-26 2014-03-19 张�成 Heavy metal sewage treating agent and preparation method thereof
JP2015231610A (en) * 2014-06-10 2015-12-24 国立大学法人山口大学 Method for processing contaminated water
CN105344318A (en) * 2015-10-30 2016-02-24 王立鑫 Active carbon composite material for water purification, and preparation method thereof

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Application publication date: 20170524