CN107551992A - A kind of method that heavy metals sorbing material is prepared using inorganic raw material - Google Patents
A kind of method that heavy metals sorbing material is prepared using inorganic raw material Download PDFInfo
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Abstract
A kind of method that heavy metals sorbing material is prepared using inorganic raw material, by potassium metaaluminate and potassium hydroxide mixed dissolution, tetraethyl oxyammonia and white carbon are added, obtains primary mixed liquor；It is put into reactor, places into baking oven, taken out after reaction, filter, wash, dry, obtain primary stage solids, be calcined, obtain primary seeds；By potassium metaaluminate and potassium hydroxide mixed dissolution, white carbon is added, obtains primary gel, ferric sulfate is added, obtains secondary gel, add primary seeds, obtain mixed gel；Mixed gel is put into reactor, crystallization is carried out in baking oven, filtering, washing, drying, obtains secondary solid；Secondary solid is added in the solution containing sodium hydroxide, carries out heating water bath；Solution is filtered, cooled down, dried, ground, 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 inorganic raw material
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 inorganic raw material, is comprised the following steps：
(1) by potassium metaaluminate and potassium hydroxide mixed dissolution in water, tetraethyl oxyammonia is then added, and stir one
The section time；
(2) white carbon is added to step (1), then obtains primary mixed liquor；
(3) the primary mixed liquor is put into stainless steel cauldron, is then placed in baking oven, taken after reacting a period of time
Go out, then filter, wash, drying, obtaining primary stage solids；
(4) primary stage solids are calcined, obtain primary seeds；
(5) by potassium metaaluminate and potassium hydroxide mixed dissolution in water, and a period of time is stirred；
(6) white carbon is added to step (5), then obtains primary gel；
(7) ferric sulfate is added into the primary gel, and stirred, obtain secondary gel；
(8) primary seeds are added into the secondary gel, and are stirred, obtain mixed gel；
(9) mixed gel is put into stainless steel cauldron, crystallization is carried out in baking oven, then filtered, wash
Wash, dry, obtain secondary solid；
(10) by the secondary solid add the solution containing sodium hydroxide in, and by the solution heating water bath condition
Under be stirred；
(11) solution after stirring is filtered, obtains whole level solid；
(12) whole level solid is cooled down；
(13) the whole level solid after step (12) is cooled down is dried；
(14) the dried whole level solid of step (13) is ground, then obtains zeolite adsorption material.
Preferably, potassium metaaluminate described in step (1) and potassium hydroxide mixed proportion are (1.5~2)：(1~1.2),
The addition of tetraethyl oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture.
Preferably, stainless steel cauldron has polytetrafluoroethylkettle kettle liner described in step (3), oven temperature is
120 DEG C~140 DEG C, react 45~48 hours.
As further preferred, sintering temperature is 500 DEG C in step (4), and roasting time is 2~3 hours.
As further preferred, potassium metaaluminate and potassium hydroxide mixed proportion are 1 in step (5):5.
Preferably, the addition of ferric sulfate is the two of step (5) potassium metaaluminate and potassium hydroxide mixture in step (7)
1/10th.
Preferably, reactor described in step (9) has polytetrafluoroethyllining lining, the temperature of baking oven is 120 DEG C~140
DEG C, crystallization 5~6 days.
As further preferred, the middle distillation water washing of step (9), and wash 4~6 times, to pH=7~7.9.
As further preferred, the concentration of sodium hydroxide is 3mol/L in step (10), and the temperature of heating water bath is 90 DEG C.
Preferably, dried described in step (13) 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 inorganic raw material
Material, zeolite quality 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：
By potassium metaaluminate and potassium hydroxide according to 1.5:1 mixed dissolution in water, then add tetraethyl oxyammonia, four
The addition of ethyl oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs a period of time, is then added
White carbon, obtain primary mixed liquor.The primary mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner
In, it is then placed in baking oven, the temperature in baking oven is 120 DEG C, and reaction is taken out after 45 hours, then filters, washs, drying, obtaining
Primary stage solids.The primary stage solids are calcined, sintering temperature is 500 DEG C, and roasting time is 2 hours, then obtains primary
Crystal seed.It is proportionally 1 by potassium metaaluminate and potassium hydroxide:5 mixed dissolutions stir a period of time in water, into solution
White carbon is added, then obtains primary gel；Ferric sulfate is added into the primary gel, the addition of ferric sulfate is inclined aluminium
Sour potassium and potassium hydroxide 1：The 20 of 5 mixtures/stir in the lump, obtain secondary gel.Institute is added into the secondary gel
Primary seeds are stated, and are stirred, obtain mixed gel；The mixed gel is put into the stainless of polytetrafluoroethyllining lining
In steel reactor, crystallization is carried out in baking oven, oven temperature is 120 DEG C, crystallization 5 days, is then filtered, and is washed 4~6 times,
To pH=7~7.9, then dry, obtain secondary solid.The secondary solid is added in the solution containing sodium hydroxide, and will
The solution is stirred under conditions of heating water bath, and wherein the concentration of sodium hydroxide is 3mol/L, and the temperature of heating water bath is
90℃.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, be dried in vacuo, ground, so
After obtain zeolite adsorption material.By the zeolite adsorption material to carrying out absorption test, adsorption rate containing heavy metal lead ion waste water
Up to more than 90%.
Embodiment 2：
By potassium metaaluminate and potassium hydroxide according to 1.5:Then 1.2 mixed dissolutions add tetraethyl oxyammonia in water,
The addition of tetraethyl oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs a period of time, is then added again
Enter white carbon, obtain primary mixed liquor.The primary mixed liquor is put into the stainless steel reaction with polytetrafluoroethylkettle kettle liner
In kettle, baking oven is then placed in, the temperature in baking oven is 130 DEG C, and reaction is taken out after 47 hours, then filters, washs, drying, obtaining
To primary stage solids.The primary stage solids are calcined, sintering temperature is 500 DEG C, and roasting time is 2.5 hours, is then obtained
Primary seeds.It is proportionally 1 by potassium metaaluminate and potassium hydroxide:5 mixed dissolutions stir a period of time, Xiang Rong in water
White carbon is added in liquid, then obtains primary gel；Ferric sulfate is added into the primary gel, the addition of ferric sulfate is
Potassium metaaluminate and potassium hydroxide 1：The 20 of 5 mixtures/stir in the lump, obtain secondary gel.Add into the secondary gel
Enter the primary seeds, and stir, obtain mixed gel；The mixed gel is put into polytetrafluoroethyllining lining
In stainless steel cauldron, crystallization is carried out in baking oven, oven temperature is 130 DEG C, crystallization 6 days, is then filtered, washing 4~6
It is secondary, to pH=7~7.9, then dry, obtain secondary solid.The secondary solid is added in the solution containing sodium hydroxide, and
The solution is stirred under conditions of heating water bath, the wherein concentration of sodium hydroxide is 3mol/L, the temperature of heating water bath
For 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, be dried in vacuo, ground,
Then zeolite adsorption material is obtained.By the zeolite adsorption material to carrying out absorption test containing heavy metal lead ion waste water, adsorb
Rate is up to more than 90%.
Embodiment 3：
By potassium metaaluminate and potassium hydroxide according to 2:Then 1 mixed dissolution adds tetraethyl oxyammonia, tetrem in water
The addition of base oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs a period of time, is then added white
Carbon black, obtain primary mixed liquor.The primary mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner,
It is then placed in baking oven, the temperature in baking oven is 140 DEG C, and reaction is taken out after 48 hours, then filters, washs, drying, obtaining primary
Solid.The primary stage solids are calcined, sintering temperature is 500 DEG C, and roasting time is 2.5 hours, then obtains primary crystalline substance
Kind.It is proportionally 1 by potassium metaaluminate and potassium hydroxide:5 mixed dissolutions stir a period of time in water, into solution again
White carbon is added, then obtains primary gel；Ferric sulfate is added into the primary gel, the addition of ferric sulfate is meta-aluminic acid
Potassium and potassium hydroxide 1：The 20 of 5 mixtures/stir in the lump, obtain secondary gel.Described in being added into the secondary gel
Primary seeds, and stir, obtain mixed gel；The mixed gel is put into the stainless steel with polytetrafluoroethyllining lining
In reactor, crystallization is carried out in baking oven, oven temperature is 140 DEG C, crystallization 6 days, is then filtered, washing 4~6 times, extremely
PH=7~7.9, then dry, obtain secondary solid.The secondary solid is added in the solution containing sodium hydroxide, and should
Solution is stirred under conditions of heating water bath, and wherein the concentration of sodium hydroxide is 3mol/L, and the temperature of heating water bath is 90
℃.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, be dried in vacuo, ground, then
Obtain zeolite adsorption material.By the zeolite adsorption material to carrying out absorption test containing heavy metal lead ion waste water, adsorption rate can
Up to more than 90%.
Embodiment 4：
By potassium metaaluminate and potassium hydroxide according to 2:1.2 mixed dissolutions in water, then add tetraethyl oxyammonia, four
The addition of ethyl oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs a period of time, is then added
White carbon, obtain primary mixed liquor.The primary mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner
In, it is then placed in baking oven, the temperature in baking oven is 140 DEG C, and reaction is taken out after 48 hours, then filters, washs, drying, obtaining
Primary stage solids.The primary stage solids are calcined, sintering temperature is 500 DEG C, and roasting time is 3 hours, then obtains primary
Crystal seed.It is proportionally 1 by potassium metaaluminate and potassium hydroxide:5 mixed dissolutions stir a period of time in water, into solution
White carbon is added, then obtains primary gel；Ferric sulfate is added into the primary gel, the addition of ferric sulfate is inclined aluminium
Sour potassium and potassium hydroxide 1：The 20 of 5 mixtures/stir in the lump, obtain secondary gel.Institute is added into the secondary gel
Primary seeds are stated, and are stirred, obtain mixed gel；The mixed gel is put into the stainless of polytetrafluoroethyllining lining
In steel reactor, crystallization is carried out in baking oven, oven temperature is 140 DEG C, crystallization 5 days, is then filtered, and is washed 4~6 times,
To pH=7~7.9, then dry, obtain secondary solid.The secondary solid is added in the solution containing sodium hydroxide, and will
The solution is stirred under conditions of heating water bath, and wherein the concentration of sodium hydroxide is 3mol/L, and the temperature of heating water bath is
90℃.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, be dried in vacuo, ground, so
After obtain zeolite adsorption material.By the zeolite adsorption material to carrying out absorption test, adsorption rate containing heavy metal lead ion waste water
Up to more than 90%.
Embodiment 5：
By potassium metaaluminate and potassium hydroxide according to 1.8:Then 1.1 mixed dissolutions add tetraethyl oxyammonia in water,
The addition of tetraethyl oxyammonia is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs a period of time, is then added again
Enter white carbon, obtain primary mixed liquor.The primary mixed liquor is put into the stainless steel reaction with polytetrafluoroethylkettle kettle liner
In kettle, baking oven is then placed in, the temperature in baking oven is 130 DEG C, and reaction is taken out after 46 hours, then filters, washs, drying, obtaining
To primary stage solids.The primary stage solids are calcined, sintering temperature is 500 DEG C, and roasting time is 2 hours, is then obtained just
Level crystal seed.It is proportionally 1 by potassium metaaluminate and potassium hydroxide:5 mixed dissolutions stir a period of time in water, to solution
In add white carbon, then obtain primary gel；Ferric sulfate is added into the primary gel, the addition of ferric sulfate is inclined
Potassium aluminate and potassium hydroxide 1：The 20 of 5 mixtures/stir in the lump, obtain secondary gel.Added into the secondary gel
The primary seeds, and stir, obtain mixed gel；The mixed gel is put into polytetrafluoroethyllining lining not
Become rusty in steel reactor, crystallization is carried out in baking oven, oven temperature is 130 DEG C, crystallization 6 days, is then filtered, washing 4~6
It is secondary, to pH=7~7.9, then dry, obtain secondary solid.The secondary solid is added in the solution containing sodium hydroxide, and
The solution is stirred under conditions of heating water bath, the wherein concentration of sodium hydroxide is 3mol/L, the temperature of heating water bath
For 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is cooled down, be dried in vacuo, ground,
Then zeolite adsorption material is obtained.By the zeolite adsorption material to carrying out absorption test containing heavy metal lead ion waste water, adsorb
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 subsequent treatment process is simple；Close
Into 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 inorganic raw material, is comprised the following steps：
(1) by potassium metaaluminate and potassium hydroxide mixed dissolution in water, when then adding tetraethyl oxyammonia, and stirring one section
Between；
(2) white carbon is added to step (1), then obtains primary mixed liquor；
(3) the primary mixed liquor is put into stainless steel cauldron, is then placed in baking oven, taken out after reacting a period of time, so
Filter, wash afterwards, drying, obtaining primary stage solids；
(4) primary stage solids are calcined, obtain primary seeds；
(5) by potassium metaaluminate and potassium hydroxide mixed dissolution in water, and a period of time is stirred；
(6) white carbon is added to step (5), then obtains primary gel；
(7) ferric sulfate is added into the primary gel, and stirred, obtain secondary gel；
(8) primary seeds are added into the secondary gel, and are stirred, obtain mixed gel；
(9) mixed gel is put into stainless steel cauldron, crystallization is carried out in baking oven, then filtered, wash, dry
It is dry, obtain secondary solid；
(10) secondary solid is added in the solution containing sodium hydroxide, and the solution is entered under conditions of heating water bath
Row stirring；
(11) solution after stirring is filtered, obtains whole level solid；
(12) whole level solid is cooled down；
(13) the whole level solid after step (12) is cooled down is dried；
(14) the dried whole level solid of step (13) is ground, then obtains zeolite adsorption material.
2. according to the method for claim 1, potassium metaaluminate described in step (1) and potassium hydroxide mixed proportion for (1.5~
2)：(1~1.2), the addition of tetraethyl oxyammonia are 3 times of potassium metaaluminate and potassium hydroxide mixture.
3. according to the method for claim 1, stainless steel cauldron has polytetrafluoroethylkettle kettle liner described in step (3),
Oven temperature is 120 DEG C~140 DEG C, is reacted 45~48 hours.
4. according to the method for claim 1, sintering temperature is 500 DEG C in step (4), roasting time is 2~3 hours.
5. according to the method for claim 1, potassium metaaluminate and potassium hydroxide mixed proportion are 1 in step (5):5.
6. according to the method for claim 1, the addition of ferric sulfate is step (5) potassium metaaluminate and hydrogen-oxygen in step (7)
Change 1st/20th of potassium mixture.
7. according to the method for claim 1, reactor has polytetrafluoroethyllining lining, the temperature of baking oven described in step (9)
Spend for 120 DEG C~140 DEG C, crystallization 5~6 days.
8. according to the method for claim 7, in step (9) with distillation water washing, and wash 4~6 times, to pH=7~
7.9。
9. according to the method for claim 1, the concentration of sodium hydroxide is 3mol/L in step (10), the temperature of heating water bath
For 90 DEG C.
10. according to the method for claim 1, dried described in step (13) as vacuum drying.
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Application publication date: 20180109 |