CN107442092A - A kind of method that hydro-thermal prepares heavy metals sorbing material - Google Patents
A kind of method that hydro-thermal prepares heavy metals sorbing material Download PDFInfo
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- CN107442092A CN107442092A CN201710775576.9A CN201710775576A CN107442092A CN 107442092 A CN107442092 A CN 107442092A CN 201710775576 A CN201710775576 A CN 201710775576A CN 107442092 A CN107442092 A CN 107442092A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—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
- B01J20/18—Synthetic zeolitic molecular sieves
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—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
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
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- 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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
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- Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract
A kind of method that hydro-thermal prepares heavy metals sorbing material, by potassium metaaluminate and potassium hydroxide mixed dissolution in water, Ludox is then added, and stir a period of time, then obtain primary mixed liquor；The primary mixed liquor is put into stainless steel cauldron, at a certain temperature reaction a period of time；The product reacted after terminating is filtered, washed, dried, obtains primary stage solids；The secondary solid is added in the solution containing ammonium chloride, and the solution is stirred under conditions of heating；Solution after stirring is filtered, obtains whole level solid；Whole level solid is cooled down；Whole level solid after cooling is dried；Dried whole level solid is 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, method that specially a kind of hydro-thermal prepares heavy metals sorbing material.
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 tri- kinds of elements of Si, Al, O, because silicon-oxy tetrahedron therein and aluminum-oxygen tetrahedron can construct infinitely
The three dimensions rack-like of extension, 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 hydro-thermal prepares heavy metals sorbing material, comprises the following steps：
(1) then potassium metaaluminate and potassium hydroxide mixed dissolution are added into Ludox in water, and stir a period of time,
Then primary mixed liquor is obtained；
(2) the primary mixed liquor is put into stainless steel cauldron, at a certain temperature reaction a period of time；
(3) product after step (2) reaction is terminated is filtered, washed, dried, and obtains primary stage solids；
(4) secondary solid is added in the solution containing ammonium chloride, and the solution is carried out under conditions of heating
Stirring；
(5) solution after stirring is filtered, obtains whole level solid；
(6) whole level solid is cooled down；
(7) the whole level solid after step (6) is cooled down is dried；
(8) the dried whole level solid of step (7) is ground, then obtains zeolite adsorption material.
Preferably, potassium metaaluminate described in step (1) and potassium hydroxide mixed proportion are (1.6~2)：(1.2~
1.5), the addition of Ludox is 3 times of potassium metaaluminate and potassium hydroxide mixture.
As further preferred, mixing time is 30min~40min in step (1).
Preferably, stainless steel cauldron described in step (2) has a polytetrafluoroethylkettle kettle liner, temperature is 150 DEG C~
200 DEG C, react 38~42 hours.
Preferably, it is filtered into suction filtration described in step (3).
Further, distillation water washing is used in step (3), and is washed 4~6 times, to pH=7~7.5.
Preferably, drying temperature is 40 DEG C in step (3).
Preferably, the concentration of ammonium chloride is 1.5mol/L in step (4).
Preferably, it is heated to be heating water bath in step (4), and the temperature of heating water bath is 90 DEG C.
Preferably, dried described in step (7) 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 hydro-thermal method
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 1.6:Then 1.2 mixed dissolutions add Ludox in water, Ludox
Addition is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs 30min, then obtains primary mixed liquor.Will be described first
Level mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner, is reacted 38 hours at being 150 DEG C in temperature；Will
Reaction terminate after product filtered, filtering from filter, then with distillation water washing, and washing 4~6 times, to pH=7~
7.5, dried at being then 40 DEG C in temperature, obtain primary stage solids.The secondary solid is added and contains the molten of ammonium chloride
In liquid, and the solution being stirred under conditions of heating, the concentration of ammonium chloride is 1.5mol/L, is heated to be heating water bath,
And the temperature of heating water bath is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is carried out cold
But, then it is dried in vacuo, then dried whole level solid is ground, then obtains zeolite adsorption material.This is boiled
Stone sorbing material containing heavy metal lead ion waste water to carrying out absorption test, and adsorption rate is up to more than 90%.
Embodiment 2：
By potassium metaaluminate and potassium hydroxide according to 1.8:Then 1.4 mixed dissolutions add Ludox in water, Ludox
Addition is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs 35min, then obtains primary mixed liquor.Will be described first
Level mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner, is reacted 40 hours at being 180 DEG C in temperature；Will
Reaction terminate after product filtered, filtering from filter, then with distillation water washing, and washing 4~6 times, to pH=7~
7.5, dried at being then 40 DEG C in temperature, obtain primary stage solids.The secondary solid is added and contains the molten of ammonium chloride
In liquid, and the solution being stirred under conditions of heating, the concentration of ammonium chloride is 1.5mol/L, is heated to be heating water bath,
And the temperature of heating water bath is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is carried out cold
But, then it is dried in vacuo, then dried whole level solid is ground, then obtains zeolite adsorption material.This is boiled
Stone sorbing material containing heavy metal lead ion waste water to carrying out absorption test, and adsorption rate is up to more than 90%.
Embodiment 3：
By potassium metaaluminate and potassium hydroxide according to 2:Then 1.5 mixed dissolutions add Ludox in water, Ludox adds
Enter 3 times that amount is potassium metaaluminate and potassium hydroxide mixture, and stir 40min, then obtain primary mixed liquor.By the primary
Mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner, is reacted 42 hours at being 200 DEG C in temperature；Will be anti-
Product after should terminating is filtered, and filtering is from filtering, then with distillation water washing, and washing 4~6 times, to pH=7~7.5,
Then dried at being 40 DEG C in temperature, obtain primary stage solids.The secondary solid is added in the solution containing ammonium chloride,
And be stirred the solution under conditions of heating, the concentration of ammonium chloride is 1.5mol/L, is heated to be heating water bath, and 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 vacuo, then dried whole level solid is ground, 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%.
Embodiment 4：
By potassium metaaluminate and potassium hydroxide according to 1.7:Then 1.4 mixed dissolutions add Ludox in water, Ludox
Addition is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs 35min, then obtains primary mixed liquor.Will be described first
Level mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner, is reacted 42 hours at being 200 DEG C in temperature；Will
Reaction terminate after product filtered, filtering from filter, then with distillation water washing, and washing 4~6 times, to pH=7~
7.5, dried at being then 40 DEG C in temperature, obtain primary stage solids.The secondary solid is added and contains the molten of ammonium chloride
In liquid, and the solution being stirred under conditions of heating, the concentration of ammonium chloride is 1.5mol/L, is heated to be heating water bath,
And the temperature of heating water bath is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is carried out cold
But, then it is dried in vacuo, then dried whole level solid is ground, then obtains zeolite adsorption material.This is boiled
Stone sorbing material containing heavy metal lead ion waste water to carrying out absorption test, and adsorption rate is up to more than 90%.
Embodiment 5：
By potassium metaaluminate and potassium hydroxide according to 1.9:Then 1.5 mixed dissolutions add Ludox in water, Ludox
Addition is 3 times of potassium metaaluminate and potassium hydroxide mixture, and stirs 35min, then obtains primary mixed liquor.Will be described first
Level mixed liquor is put into the stainless steel cauldron with polytetrafluoroethylkettle kettle liner, is reacted 42 hours at being 200 DEG C in temperature；Will
Reaction terminate after product filtered, filtering from filter, then with distillation water washing, and washing 4~6 times, to pH=7~
7.5, dried at being then 40 DEG C in temperature, obtain primary stage solids.The secondary solid is added and contains the molten of ammonium chloride
In liquid, and the solution being stirred under conditions of heating, the concentration of ammonium chloride is 1.5mol/L, is heated to be heating water bath,
And the temperature of heating water bath is 90 DEG C.Solution after stirring is filtered, obtains whole level solid, whole level solid is carried out cold
But, then it is dried in vacuo, then dried whole level solid is ground, then obtains zeolite adsorption material.This is boiled
Stone sorbing 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 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 hydro-thermal prepares heavy metals sorbing material, comprises the following steps：
(1) then potassium metaaluminate and potassium hydroxide mixed dissolution are added into Ludox in water, and stirs a period of time, then
Obtain primary mixed liquor；
(2) the primary mixed liquor is put into stainless steel cauldron, at a certain temperature reaction a period of time；
(3) product after step (2) reaction is terminated is filtered, washed, dried, and obtains primary stage solids；
(4) secondary solid is added in the solution containing ammonium chloride, and the solution is stirred under conditions of heating；
(5) solution after stirring is filtered, obtains whole level solid；
(6) whole level solid is cooled down；
(7) the whole level solid after step (6) is cooled down is dried；
(8) the dried whole level solid of step (7) 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 (1.6~
2)：(1.2~1.5), the addition of Ludox are 3 times of potassium metaaluminate and potassium hydroxide mixture.
3. method according to claim 1 or 2, mixing time is 30min~40min in step (1).
4. according to the method for claim 1, stainless steel cauldron has polytetrafluoroethylkettle kettle liner described in step (2),
Temperature is 150 DEG C~200 DEG C, is reacted 38~42 hours.
5. according to the method for claim 1, step is filtered into suction filtration described in (3).
6. method according to claim 1 or 5, with distillation water washing in step (3), and wash 4~6 times, to pH=7~
7.5。
7. according to the method for claim 6, drying temperature is 40 DEG C in step (3).
8. according to the method for claim 1, the concentration of ammonium chloride is 1.5mol/L in step (4).
9. according to the method for claim 8, it is heated to be heating water bath in step (4), and the temperature of heating water bath is 90 DEG C.
10. according to the method for claim 1, dried described in step (7) as vacuum drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710775576.9A CN107442092A (en) | 2017-08-31 | 2017-08-31 | A kind of method that hydro-thermal prepares heavy metals sorbing material |
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| CN201710775576.9A CN107442092A (en) | 2017-08-31 | 2017-08-31 | A kind of method that hydro-thermal prepares heavy metals sorbing material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108393065A (en) * | 2018-03-06 | 2018-08-14 | 江苏开放大学（江苏城市职业学院） | A kind of fly ash float Compound Heavy Metals sorbing material and its application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228826A (en) * | 2011-04-13 | 2011-11-02 | 北京化工大学 | Porous heterogeneous mesoporous acidic material and preparation method thereof |
| CN102923807A (en) * | 2012-09-28 | 2013-02-13 | 珠海市吉林大学无机合成与制备化学重点实验室 | Application of low-silicon micro-pore NaA type and NaX type molecular sieves in treatment of low-concentration heavy metal ions |
| CN104876354A (en) * | 2015-05-26 | 2015-09-02 | 福州大学 | Process for treatment of PTA refining wastewater through high-selectivity adsorbent |
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2017
- 2017-08-31 CN CN201710775576.9A patent/CN107442092A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228826A (en) * | 2011-04-13 | 2011-11-02 | 北京化工大学 | Porous heterogeneous mesoporous acidic material and preparation method thereof |
| CN102923807A (en) * | 2012-09-28 | 2013-02-13 | 珠海市吉林大学无机合成与制备化学重点实验室 | Application of low-silicon micro-pore NaA type and NaX type molecular sieves in treatment of low-concentration heavy metal ions |
| CN104876354A (en) * | 2015-05-26 | 2015-09-02 | 福州大学 | Process for treatment of PTA refining wastewater through high-selectivity adsorbent |
Non-Patent Citations (2)
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| 赵临襄等: "《化学制药工艺学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108393065A (en) * | 2018-03-06 | 2018-08-14 | 江苏开放大学（江苏城市职业学院） | A kind of fly ash float Compound Heavy Metals sorbing material and its application |
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