CN107551993A - A kind of method that heavy metals sorbing material is prepared using Organic Ingredients - Google Patents
A kind of method that heavy metals sorbing material is prepared using Organic Ingredients Download PDFInfo
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- CN107551993A CN107551993A CN201710775581.XA CN201710775581A CN107551993A CN 107551993 A CN107551993 A CN 107551993A CN 201710775581 A CN201710775581 A CN 201710775581A CN 107551993 A CN107551993 A CN 107551993A
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Abstract
The present invention relates to a kind of method that heavy metals sorbing material is prepared using Organic Ingredients, by silicon source and alkali mixed dissolution in water, adds silicon source, is then aged, and adds cationic polymer, and stir；Aluminum sulfate is added, gel is obtained after stirring；Gel is put into reactor and carries out crystallization for a period of time；Product after crystallization filtered, wash after be dried；Then calcining a period of time, secondary solid is obtained；Secondary solid is added in the solution containing sodium hydroxide, and the solution is stirred under conditions of heating water bath；Solution after stirring is filtered, obtains whole level solid；Whole level solid is cooled down, is ground after drying, then obtains zeolite adsorption material.Preparation technology of the present invention is simple, and reaction condition easily reaches, green, and energy consumption is small, and zeolite adsorption material purity is high, advantages of good adsorption effect.
Description
Technical field
The present invention relates to field of Environment Protection, specially a kind of side that heavy metals sorbing material is prepared using Organic Ingredients
Method.
Background technology
With the continuous development of human society, while economic development brings benefit, many pollutions are also generated.Industry
" three wastes " increase severely and the increase of vehicle exhaust discharge quantity, heavy metal in the soil, water body and plant in environment for human survival
Pollution is on the rise, and turns into economic, society and the ecological problem shown especially in harmonious development.Heavy metal typically can not be biological
Degraded, once into being difficult to remove if in water body or soil, human body can be entered by food chain approach so as to cause many diseases
The generation of (such as cancer).
Absorption method is a kind of effective physical chemistry method for treating water, is commonly used for purification of heavy metal pollution waste water.Zeolite
The tetrahedron being made up of Si, Al, O3 kind element, because silicon-oxy tetrahedron therein and aluminum-oxygen tetrahedron can construct unlimited expansion
The three dimensions rack-like of exhibition, therefore zeolite has very strong absorption and ion-exchange capacity.
Find that the adsorption phenomena in " charcoal-gas " system is come from latter stage in 18th century, adsorption operations are widely used in gas
Body separates and purified industrial.Nineteen thirties, foreign countries start to carry out zeolite systematic research, and first using natural
Chabasie is as adsorbent separation gas, liquid mixture.As artificial synthetic zeolite's molecular sieve is as adsorbent exploitation and profit
With large-scale absorbing unit operation is widely used among industrial practice.The particularly isolation technics such as PSA, TSA and VSA
Appearance greatly promoted adsorbing separation industrial expansion.And adsorbent is then the basis of PSA, TSA and VSA isolation technics,
The performance of adsorbent directly affects separating effect.Although occur organic resin, carbon molecular sieve, pillared clays etc. in recent years
Adsorbent, but zeolite molecular sieve by its regular crystal structure and can modulation surface nature, still adsorbing separation industry
Dominate, have broad application prospects.
Zeolite molecular sieve is the aluminosilicate of the cage type hole skeleton of natural or artificial synthesized alkali metal containing or alkaline-earth metal
Salt crystal material, is typically referred to as zeolite (zeolite) by natural molecular sieve, and artificial synthesized is referred to as molecular sieve
(molecular), both chemical compositions and molecular structure have no essential distinction, therefore are commonly referred to as zeolite molecular sieve.Zeolite molecules
Sieve has strict structure and space, and pore size is because architectural difference is slightly changed, it is achieved thereby that to different molecular size thing
The separation of matter.
But existing zeolite molecular sieve synthesis cost is higher, the synthetic yield of zeolite molecular sieve is relatively low, so needing
New, green Zeolite synthesis route is explored, is directed to reducing the synthesis cost of molecular screen material, finds in Zeolite synthesis
New breakthrough, application of the molecular sieve in industrial circle is promoted significantly.
The content of the invention
The shortcomings that for above-mentioned prior art, the present invention provide a kind of system of zeolite adsorption material green, cost is low
Preparation Method.
The present invention solves above-mentioned technical problem and uses following technical scheme：
A kind of method that heavy metals sorbing material is prepared using Organic Ingredients, is comprised the following steps：
(1) by silicon source and alkali mixed dissolution in water, and a period of time is stirred；
(2) silicon source is added to step (1), then obtains primary mixed liquor；
(3) the primary mixed solution is aged；
(4) cationic polymer is added in solution after being aged to step (3), and is stirred；
(5) aluminum sulfate is added to step (4) resulting solution, gel is obtained after stirring；
(6) gel is put into reactor and carries out crystallization for a period of time；
(7) product after crystallization in step (6) is filtered, obtains filtering primary stage solids；
(8) primary stage solids are washed；
(9) primary stage solids after washing are dried；
(10) solid calcining a period of time, obtains secondary solid after drying；
(11) by the secondary solid add the solution containing sodium hydroxide in, and by the solution heating water bath condition
Under be stirred；
(12) solution after stirring is filtered, obtains whole level solid；
(13) whole level solid is cooled down；
(14) the whole level solid after step (13) is cooled down is dried；
(15) the dried whole level solid of step (14) is ground, then obtains zeolite adsorption material.
Preferably, silicon source described in rapid (1) is potassium aluminate, alkali is potassium hydroxide, the mixing of potassium aluminate and potassium hydroxide
Ratio is (1~1.5):(5~6)；The water is deionized water, stirs 30min.
Preferably, silicon source described in step (2) is sodium metasilicate, addition speed is 1mL/min, in the primary mixed liquor
Aluminum oxide, potassium oxide, the ratio of silica are 1：(15~16)：(8~9).
As further preferred, digestion time described in step (3) is 24~36 hours.
As further preferred, cationic polymer described in step (4) is diallyl dimethyl ammonium chloride, stirring
Uniformly.
Preferably, reactor has polytetrafluoroethyllining lining described in step (6), at 100~120 DEG C crystallization 8~
11 days.
Preferably, using distillation water washing in step (8), and wash 4~6 times, to pH=7~7.9.
Preferably, calcining heat described in step (10) is 500 DEG C, 2h is calcined.
Preferably, the concentration of sodium hydroxide is 3mol/L in step (11), the temperature of heating water bath is 90 DEG C.
Preferably, dried described in step (14) as vacuum drying.
The present invention has the following advantages that compared with prior art：Present invention process is simple, and reaction condition easily reaches, reaction
Also easy to control, aftertreatment technology is simple；Raw material sources of the present invention are wide, and cost is low, and impurity content is low, final products impurity content
Small, purity is high；Synthetic ratio of the present invention is high, and technological process is green, and energy consumption is small；The present invention prepares zeolite material using organic formwork
Material, zeolite pore-forming effect is good, and heavy metal adsorption rate is also high, and overall production cost is low, it is easy to accomplish industrial-scale production.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.It should be appreciated that specific embodiment described herein is only explaining this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1：
Potassium aluminate is selected to select potassium hydroxide as alkali as silicon source；It is 1 in proportion by potassium aluminate and potassium hydroxide:5 is mixed
Close, be then dissolved in deionized water, and stir 30min.Then silicon source sodium metasilicate is added, addition speed is 1mL/min, so
After obtain primary mixed liquor, aluminum oxide, potassium oxide, the ratio of silica are 1 in primary mixed liquor：15：8.Primary mixed liquor is entered
Row ageing 24 hours, then adds cationic polymer diallyl dimethyl ammonium chloride into solution after ageing, and stirring is equal
It is even, aluminum sulfate is then added, gel is obtained after stirring；The gel is put into the reactor with polytetrafluoroethyllining lining
In, crystallization is carried out at 100 DEG C 8 days.Product after crystallization is filtered, obtains filtering primary stage solids, by institute
Primary stage solids are stated to be washed, with distillation water washing, and wash 4~6 times, to pH=7~7.9.Primary stage solids after washing are entered
Row drying, 2h is calcined at being then 500 DEG C in calcining heat, obtains secondary solid；The secondary solid is added and contains hydrogen-oxygen
In the solution for changing sodium, and the solution is stirred under conditions of heating water bath, the concentration of sodium hydroxide is 3mol/L, water-bath
The temperature of heating is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, then
It is dried in vacuum, dried whole level solid is ground, and then obtains zeolite adsorption material.By the zeolite adsorption material
To carrying out absorption test containing heavy metal lead ion waste water, adsorption rate is up to more than 90%.
Embodiment 2：
Potassium aluminate is selected to select potassium hydroxide as alkali as silicon source；It is 1 in proportion by potassium aluminate and potassium hydroxide:6 is mixed
Close, be then dissolved in deionized water, and stir 30min.Then silicon source sodium metasilicate is added, addition speed is 1mL/min, so
After obtain primary mixed liquor, aluminum oxide, potassium oxide, the ratio of silica are 1 in primary mixed liquor：15：9.Primary mixed liquor is entered
Row ageing 30 hours, then adds cationic polymer diallyl dimethyl ammonium chloride into solution after ageing, and stirring is equal
It is even, aluminum sulfate is then added, gel is obtained after stirring；The gel is put into the reactor with polytetrafluoroethyllining lining
In, crystallization is carried out at 110 DEG C 10 days.Product after crystallization is filtered, obtains filtering primary stage solids, by institute
Primary stage solids are stated to be washed, with distillation water washing, and wash 4~6 times, to pH=7~7.9.Primary stage solids after washing are entered
Row drying, 2h is calcined at being then 500 DEG C in calcining heat, obtains secondary solid；The secondary solid is added and contains hydrogen-oxygen
In the solution for changing sodium, and the solution is stirred under conditions of heating water bath, the concentration of sodium hydroxide is 3mol/L, water-bath
The temperature of heating is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, then
It is dried in vacuum, dried whole level solid is ground, and then obtains zeolite adsorption material.By the zeolite adsorption material
To carrying out absorption test containing heavy metal lead ion waste water, adsorption rate is up to more than 90%.
Embodiment 3：
Potassium aluminate is selected to select potassium hydroxide as alkali as silicon source；It is 1.5 in proportion by potassium aluminate and potassium hydroxide:5
Mixing, is then dissolved in deionized water, and stir 30min.Then silicon source sodium metasilicate is added, addition speed is 1mL/min,
Then primary mixed liquor is obtained, aluminum oxide, potassium oxide, the ratio of silica are 1 in primary mixed liquor：16：9.By primary mixed liquor
Ageing 36 hours is carried out, cationic polymer diallyl dimethyl ammonium chloride, stirring are then added into solution after ageing
Uniformly, aluminum sulfate is then added, gel is obtained after stirring；The gel is put into the reactor with polytetrafluoroethyllining lining
In, crystallization is carried out at 120 DEG C 11 days.Product after crystallization is filtered, obtains filtering primary stage solids, by institute
Primary stage solids are stated to be washed, with distillation water washing, and wash 4~6 times, to pH=7~7.9.Primary stage solids after washing are entered
Row drying, 2h is calcined at being then 500 DEG C in calcining heat, obtains secondary solid；The secondary solid is added and contains hydrogen-oxygen
In the solution for changing sodium, and the solution is stirred under conditions of heating water bath, the concentration of sodium hydroxide is 3mol/L, water-bath
The temperature of heating is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, then
It is dried in vacuum, dried whole level solid is ground, and then obtains zeolite adsorption material.By the zeolite adsorption material
To carrying out absorption test containing heavy metal lead ion waste water, adsorption rate is up to more than 90%.
Embodiment 4：
Potassium aluminate is selected to select potassium hydroxide as alkali as silicon source；It is 1.5 in proportion by potassium aluminate and potassium hydroxide:6
Mixing, is then dissolved in deionized water, and stir 30min.Then silicon source sodium metasilicate is added, addition speed is 1mL/min,
Then primary mixed liquor is obtained, aluminum oxide, potassium oxide, the ratio of silica are 1 in primary mixed liquor：16：8.By primary mixed liquor
Ageing 32 hours is carried out, cationic polymer diallyl dimethyl ammonium chloride, stirring are then added into solution after ageing
Uniformly, aluminum sulfate is then added, gel is obtained after stirring；The gel is put into the reactor with polytetrafluoroethyllining lining
In, crystallization is carried out at 120 DEG C 9 days.Product after crystallization is filtered, obtains filtering primary stage solids, by institute
Primary stage solids are stated to be washed, with distillation water washing, and wash 4~6 times, to pH=7~7.9.Primary stage solids after washing are entered
Row drying, 2h is calcined at being then 500 DEG C in calcining heat, obtains secondary solid；The secondary solid is added and contains hydrogen-oxygen
In the solution for changing sodium, and the solution is stirred under conditions of heating water bath, the concentration of sodium hydroxide is 3mol/L, water-bath
The temperature of heating is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, then
It is dried in vacuum, dried whole level solid is ground, and then obtains zeolite adsorption material.By the zeolite adsorption material
To carrying out absorption test containing heavy metal lead ion waste water, adsorption rate is up to more than 90%.
Embodiment 5：
Potassium aluminate is selected to select potassium hydroxide as alkali as silicon source；It is 1 in proportion by potassium aluminate and potassium hydroxide:6 is mixed
Close, be then dissolved in deionized water, and stir 30min.Then silicon source sodium metasilicate is added, addition speed is 1mL/min, so
After obtain primary mixed liquor, aluminum oxide, potassium oxide, the ratio of silica are 1 in primary mixed liquor：15.5：8.5.Primary is mixed
Liquid carries out ageing 28 hours, and cationic polymer diallyl dimethyl ammonium chloride is then added into solution after ageing, is stirred
Mix uniformly, then add aluminum sulfate, gel is obtained after stirring；The gel is put into the reaction with polytetrafluoroethyllining lining
In kettle, crystallization is carried out at 120 DEG C 10 days.Product after crystallization is filtered, obtains filtering primary stage solids, will
The primary stage solids are washed, with distillation water washing, and wash 4~6 times, to pH=7~7.9.Primary stage solids after washing
It is dried, calcines 2h at being then 500 DEG C in calcining heat, obtain secondary solid；The secondary solid is added and contains hydrogen
In the solution of sodium oxide molybdena, and the solution is stirred under conditions of heating water bath, the concentration of sodium hydroxide is 3mol/L, water
The temperature of bath heating is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, then
It is dried in a vacuum, dried whole level solid is ground, and then obtains zeolite adsorption material.By the zeolite adsorption material
Material containing heavy metal lead ion waste water to carrying out absorption test, and adsorption rate is up to more than 90%.
Preparation technology of the present invention is simple, and reaction condition easily reaches, and reaction is also easy to control, and aftertreatment technology is simple；Synthesis
Zeolite adsorption material purity it is high, impurity content is few.It is good to adsorb heavy metal effect；Drying process is simple, and energy consumption is small.
The general principle and principal character and advantages of the present invention of the present invention, the technology of the industry has been shown and described above
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention, the claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of method that heavy metals sorbing material is prepared using Organic Ingredients, is comprised the following steps：
(1) by silicon source and alkali mixed dissolution in water, and a period of time is stirred；
(2) silicon source is added to step (1), then obtains primary mixed liquor；
(3) the primary mixed solution is aged；
(4) cationic polymer is added in solution after being aged to step (3), and is stirred；
(5) aluminum sulfate is added to step (4) resulting solution, gel is obtained after stirring；
(6) gel is put into reactor and carries out crystallization for a period of time；
(7) product after crystallization in step (6) is filtered, obtains filtering primary stage solids；
(8) primary stage solids are washed；
(9) primary stage solids after washing are dried；
(10) solid calcining a period of time, obtains secondary solid after drying；
(11) secondary solid is added in the solution containing sodium hydroxide, and the solution is entered under conditions of heating water bath
Row stirring；
(12) solution after stirring is filtered, obtains whole level solid；
(13) whole level solid is cooled down；
(14) the whole level solid after step (13) is cooled down is dried；
(15) the dried whole level solid of step (14) is ground, then obtains zeolite adsorption material.
2. according to the method for claim 1, silicon source described in step (1) be potassium aluminate, alkali is potassium hydroxide, potassium aluminate and
The mixed proportion of potassium hydroxide is (1~1.5):(5~6)；The water is deionized water, stirs 30min.
3. according to the method for claim 1, silicon source described in step (2) is sodium metasilicate, addition speed is 1mL/min, institute
It is 1 to state aluminum oxide in primary mixed liquor, potassium oxide, the ratio of silica：(15~16)：(8~9).
4. according to the method for claim 1, digestion time described in step (3) is 24~36 hours.
5. according to the method for claim 1, cationic polymer described in step (4) is diallyl dimethyl chlorination
Amine, stir.
6. according to the method for claim 1, reactor has polytetrafluoroethyllining lining described in step (6), 100~
Crystallization 8~11 days at 120 DEG C.
7. according to the method for claim 1, in step (8) with distillation water washing, and wash 4~6 times, to pH=7~
7.9。
8. according to the method for claim 1, calcining heat described in step (10) is 500 DEG C, 2h is calcined.
9. according to the method for claim 1, the concentration of sodium hydroxide is 3mol/L in step (11), the temperature of heating water bath
For 90 DEG C.
10. according to the method for claim 1, dried described in step (14) as vacuum drying.
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| CN109824110A (en) * | 2019-02-28 | 2019-05-31 | 长沙埃比林环保科技有限公司 | A kind of preparation method of heavy metal containing sewage adsorbent material |
| CN109824111A (en) * | 2019-02-28 | 2019-05-31 | 长沙埃比林环保科技有限公司 | A kind of preparation method of sewage adsorbent material |
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| CN109824110A (en) * | 2019-02-28 | 2019-05-31 | 长沙埃比林环保科技有限公司 | A kind of preparation method of heavy metal containing sewage adsorbent material |
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Application publication date: 20180109 |