CN108517563A - A kind of layered double hydroxide LDH-Cl2-I2Whisker and its preparation method and application - Google Patents
A kind of layered double hydroxide LDH-Cl2-I2Whisker and its preparation method and application Download PDFInfo
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- CN108517563A CN108517563A CN201810297649.2A CN201810297649A CN108517563A CN 108517563 A CN108517563 A CN 108517563A CN 201810297649 A CN201810297649 A CN 201810297649A CN 108517563 A CN108517563 A CN 108517563A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The present invention relates to a kind of layered double hydroxide LDH Cl2‑I2Whisker and its preparation method and application.The chemical formula of the whisker is Mg6Al2(OH)14Cl2I2·4H2O;The whisker passes through metal cation Mg2+And Al3+With anion Cl‑、I‑And OH‑Evaporable water obtains after reacting to precipitate.Layered double hydroxide LDH Cl provided by the invention2‑I2Whisker is a kind of houghite compound of crystal whisker-shaped, in addition to the classes talcs compounds such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeability with aperture, also has the function of crystal whisker toughened reinforcement, there is very extensive application prospect in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material.Preparation method provided by the invention, it is simple for process, it is suitble to large-scale promotion.
Description
Technical field
The invention belongs to Material Fields, more particularly, to a kind of layered double hydroxide LDH-Cl2-I2Whisker and
Preparation method and application.
Background technology
Layered double hydroxide (Layered Double Hydroxide, LDH) is hydrotalcite
The general designation of (Hydrotalcite, HT) and houghite compound (Hydrotalcite-Like Compounds, HTLc) is
A kind of important inorganic functional material has the function of catalysis, absorption, fire-retardant etc., is a kind of multifunctional inorganic material of environment-friendly type.
Most typical LDH is Mg6Al2(OH)16CO3·4H2O, also referred to as magnalium hydrotalcite, if in this magnalium hydrotalcite
Mg2+、A13+Or CO3 2-Ion is replaced by other ions, you can obtains houghite (HTLc).The general formula of HTLc is:(m=0,1,2N) (wherein M2+For bivalent metal ion, such as Mg2+、Ni2+、
Co2+、Zn2+、Cu2+Deng;M3+For trivalent metal ion, such as Al3+、Cr3+、Fe3+、Sc3+Deng;A is interlayer anion, such as CO3 2-、
NO3-、Cl-、 SO4 2-、PO4 3-、C6H4(COO)2 2-Deng;M be Coating combination water number mesh) byIt is formed
Plate layer is known as sheet-metal layers, byThe layer of composition is known as anion layer.This layer structure can indicate as follows:
Since HTLc has the adjustable denaturation in aperture, and there are larger specific surface area and interlayer ion interchangeability, therefore its
There is very extensive application prospect in the fields such as catalysis, fire-retardant, absorption, medicine, gene storage.
For LDH, HTLc class compound, the research that domestic and international many is engaged in this respect at present is done a lot of work, and
Gratifying achievement is all achieved in respective field.It is both domestic and external to study the displacement for being concentrated mainly on sheet-metal layers bivalent cation
On, such as magnesium ion is replaced into copper ion or cobalt ions etc., anion metathesis is some such as amino acid by the design also having
Equal organic biomolecules.At home, Beijing University of Chemical Technology achieves prodigious achievement to the research of LDH.They contain in design
Prodigious achievement in research is achieved in the intercalations LDH field of compound material such as copper, cobalt, nickel, organic acid, polyacid.At abroad, also having
Many scholars synthesize numerous important organic compounds and inorganization on preparing LDH technologies or using LDH as catalyst
It closes on object or as many gratifying achievements are also achieved in the researchs such as fire retardant, adsorbent, provides a large amount of useful
Experimental data.But extremely currently, LDH and HTLc class compounds are mainly laminated structure, LDH the and HTLc class compounds of crystal whisker-shaped
Almost without report.And the inorganic material of crystal whisker-shaped has toughened and reinforced function, can such as develop LDH the or HTLc classes of crystal whisker-shaped
Closing object can then assign LDH and HTLc classes inorganic material preferably toughened and reinforced function, further to widen its application.
Therefore, developing a kind of LDH and/or HTLc class compounds of crystal whisker-shaped has great research significance and application value.
Invention content
Present invention aims at the research blank for the LDH and HTLc class compounds for making up crystal whisker-shaped in the prior art, provide
A kind of layered double hydroxide LDH-Cl2-I2Whisker.Layered double hydroxide LDH-Cl provided by the invention2-I2
Whisker removes the work(of the classes talcs compounds such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeability with aperture
Can be outer, it is non-also to have the function of that crystal whisker toughened reinforcement has in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material
Often it is widely applied foreground.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl2-I2The preparation side of whisker
Method.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl2-I2Whisker is preparing toughening
Application in supporting material, catalysis material, fire proofing or sorbing material.
For achieving the above object, the present invention adopts the following technical scheme that:
A kind of layered double hydroxide LDH-Cl2-I2The chemical formula of whisker, the whisker is Mg6Al2(OH)14Cl2I2·4H2O;The whisker passes through metal cation Mg2+And Al3+With anion Cl-、 I-And OH-It is steamed after reacting to precipitate
Shampoo is got.
The present invention provides a kind of layered double hydroxide LDH-Cl of specific composition2-I2Whisker, the substance are crystalline substance
The draw ratio of palpus shape, whisker is 15~25:1, good dispersion, whisker crystal form is good, has toughened and reinforced caused by whisker structure
Function;Adjustable denaturation, larger specific surface area and layer of the substance again with aperture possessed by HTLc class compounds simultaneously
Between ion interchangeability function, have in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material very extensive
Application prospect.
The present invention provides a kind of above-mentioned layered double hydroxide LDH-Cl2-I2The preparation method of whisker, the preparation
Method includes the following steps:
S1:Prepare MgI2And AlCl3Mixed solution, be adjusted to NaOH the or KOH solution of 0.0085~0.0115mol/L
PH is 7.45~7.55;Mg in the mixed solution2+A concentration of 2.1~2.7mol/L, Al3+A concentration of 0.65~
0.95mol/L;
S2:Be added into mixed solution 0.0085~0.0115mol/L NaOH or KOH solution to pH be 7.95~8.05
Afterwards, reaction generates precipitation;
S3:Precipitation obtained by S2 is placed at 5~45 DEG C evaporable water to get layered double-metal hydroxide LDH-
Cl2-I2Whisker.
The present invention is to layered double hydroxide LDH-Cl2-I2Preparation process explore it is found that raw material and its matching
There is significant impact to the pattern of final layered double hydroxide than, pH regulation and control and temperature regulation and control.Such as metal cation Mg2+
And Al3+, anion Cl-、I-And OH-Concentration it is excessive or too small, pH is excessively high or pH fluctuation ranges are excessive, temperature when moisture evaporation
Excessively high (water evaporation rate is too fast) be unable to get whisker morphology or obtain whisker morphology yield it is very low.The present invention passes through
This series of conditions it is preferred, finally prepare the layered double hydroxide LDH-Cl of crystal whisker-shaped2-I2, preparation method letter
It is single.
In addition, Qinghai Salt Lake (such as Hoh Yanhu bittern, Chaka Salt lake bittern or Cha Er Han Salt Lake) has the hardship of enormous amount
Halogen, these bitterns are to prepare LDH-Cl2-I2The extremely excellent natural resources of whisker.But these resources cannot get always science, high level profit
With, but leave unused always, this not only wastes salt lake resources, also so that the serious salination of salt lake Soil Surrounding and plant are withered
Extremely, it is damaged to the ecological environment in salt lake, while also bringing difficulty to saltern resource exploitation in future.Using bittern in salt lake as
Mg2+And Cl-Source, the natural resources can be made full use of, it is cost-effective, have important economic value.
Preferably, the MgI2And AlCl3From Qinghai Salt Lake bittern.It is further preferable that the MgI2And AlCl3Come
Derived from Cha Er Han Salt Lake bittern.
Preferably, it is 7.5 that pH is adjusted in S1.
Preferably, Mg in S1 mixed solutions2+A concentration of 2.4mol/L;Al in S1 mixed solutions3+It is a concentration of
0.8mol/L。
Preferably, NaOH described in the S2 or a concentration of 0.01mol/L of KOH solution.
Preferably, be added in S2 NaOH or KOH solution to pH be 8.00.
Preferably, the reaction time of S2 is 95~101h.
It is further preferable that the reaction time of S2 is 98h.
In order to preferably regulate and control pH, prevent pH too low or fluctuation be excessive, it is preferable that in S2 per 6h by add NaOH or
KOH solution adjusts the pH of mixed solution, and the changing value for adding the pH before and after NaOH or KOH solution every time is not more than 0.05.
Preferably, the NaOH of the pH for adjusting mixed solution or a concentration of 0.0085~0.0115mol/ of KOH solution
L。
In order to enable moisture evaporation is more uniformly distributed, it is preferable that further including wind step in S3 makes moisture evaporation, the wind
Wind speed be 4~5m/s.
Qinghai Salt Lake area has abundant solar energy resources and wind energy resources, and long-term temperature is at 5~45 DEG C, and wind speed is 4
Precipitation obtained by S2 can be placed at the spaciousness of Qinghai Salt Lake area, water is realized using natural solar energy and wind energy resources by~5m/s
Divide slow evaporation, not only saves energy and realize green chemical industry.
Above-mentioned layered double hydroxide LDH-Cl2-I2Whisker is preparing toughened and reinforced material, catalysis material, fire-retardant material
Application in material or sorbing material is also within the scope of the present invention.
Compared with prior art, the present invention has the advantages that:
Layered double hydroxide LDH-Cl provided by the invention2-I2Whisker is a kind of houghite chemical combination of crystal whisker-shaped
Object had not only had the function of crystal whisker toughened reinforcement, but also had adjustable denaturation, larger specific surface area and the interlayer ion in aperture commutative
Property etc. classes talcs compound function, have in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material very wide
General application prospect.Preparation method provided by the invention, it is simple for process, it is suitble to large-scale promotion.
Description of the drawings
Fig. 1 is that embodiment 1 prepares layered double hydroxide LDH-Cl2-I2The route map of whisker;
Fig. 2 is the layered double hydroxide LDH-Cl that embodiment 1 provides2-I2The shape appearance figure of whisker;
Fig. 3 is the layered double hydroxide LDH-Cl that the embodiment of the present invention 1 provides2-I2The XRD of whisker schemes;
Fig. 4 is the shape appearance figure of sample prepared by comparative example 1 of the present invention.
Specific implementation mode
With reference to embodiment, the present invention will be further described.These embodiments are retouched to the typical case of the present invention
It states, however, the present invention is not limited thereto.Test method as used in the following examples is conventional method unless otherwise specified;Made
Raw materials and reagents etc. are unless otherwise specified that can be commercially available from conventional commercial sources.
Embodiment 1
The present embodiment provides a kind of layered double hydroxide LDH-Cl2-I2Whisker, chemical formula Mg6Al2
(OH)14Cl2I2·4H2O, preparation method are following (such as Fig. 1):
S1:Prepare 4.80molL-1MgI2·8H2O and 1.6molL-1AlCl3·6H2O solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01mol/L
=7.50, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with follow-up LDH-
Cl2-I2The growth of whisker.
S2:The NaOH solution for preparing 0.010mol/L, is added to while stirring in the mixed liquor obtained by two steps, adds always
To the pH to pH=8.00 of system.Then by system be placed in sun-drenched place allow expose to the weather 98h (temperature be 5~45 DEG C,
Wind speed is 4~5m/s) after, precipitation is filtered and washed, is dried to get sample.In the time of this 98h, one was added every 6 hours
The NaOH solution of secondary 0.010mol/L, the amount being added every time are:The pH value for first measuring current arrangements, is then added NaOH so that
PH value increase by 0.05 unit, for example, measure at this time system pH be 7.25, then be added alkali when be added to system pH always
Terminate when being 7.30.
The layered double hydroxide LDH-Cl that the present embodiment is prepared2-I2The draw ratio of whisker is 15~25:1,
Good dispersion, whisker good crystalline have preferable toughened and reinforced function, such as Fig. 1;In addition, can from its XRD diffraction pattern (such as Fig. 2)
To find out, layered double hydroxide LDH-Cl2-I2(LDH's layer structure of the compound with LDH of layer structure exists
(003) crystal face diffracted intensity is maximum, followed by (006) crystal face, and minimum is (009), this is because lamellar compound is to XRD
" delustring " effect caused by.
Whisker manufactured in the present embodiment is prepared into sample and carries out elemental analysis, elemental analysis of samples result acquired results row
In table 1, table 1 statistics indicate that, embodiment 1 provide sample substantially conform to nMg:nAl:ncl:nI=3:1:1:1, in conjunction with oxygen (oxygen
Content is obtained by minusing), protium content, can deduce its chemical formula be Mg6Al2(OH)14Cl2I2·4H2O。
1 LDH-Cl of table2-I2Elemental analysis result
Embodiment 2
The present embodiment provides a kind of layered double hydroxide LDH-Cl2-I2Whisker, chemical formula Mg6Al2(OH)14Cl2I2·4H2O, preparation method are as follows:
S1:Prepare 4.20molL-1MgI2·8H2O and 1.9molL-1AlCl3·6H2O solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to the NaOH solution of 0.0085mol/L
PH=7.45, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with subsequently
LDH-Cl2-I2The growth of whisker.
S2:The NaOH solution for preparing 0.0085mol/L, is added in the mixed liquor obtained by two steps, always while stirring
Add to the pH to pH=7.95 of system.Then by system be placed in sun-drenched place allow expose to the weather 101h (temperature be 5~45
DEG C, wind speed is 4~5m/s) after, precipitation is filtered and washed, is dried to get sample.In the time of this 101h, added every 6 hours
The NaOH solution for entering a 0.0085mol/L, the amount being added every time are:The pH value for first measuring current arrangements, is then added NaOH,
So that pH value increase by 0.05 unit, for example, measure at this time system pH be 7.15, then be added alkali when be added to system always
PH value terminates when being 7.20.
The layered double hydroxide LDH-Cl that the present embodiment is prepared2-I2The draw ratio of whisker is 15~25:1,
Good dispersion, whisker good crystalline, XRD diffraction patterns have the diffractive features of LDH.Therefore, it is the whisker with LDH structures.
Embodiment 3
The present embodiment provides a kind of layered double hydroxide LDH-Cl2-I2Whisker, chemical formula Mg6Al2
(OH)14Cl2I2·4H2O, preparation method are as follows:
S1:Prepare 5.4molL-1MgI2·8H2O and 1.3molL-1AlCl3·6H2O solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to the NaOH solution of 0.0115mol/L
PH=7.55, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with subsequently
LDH-Cl2-I2The growth of whisker.
S2:The NaOH solution for preparing 0.0115mol/L, is added in the mixed liquor obtained by two steps, always while stirring
Add to the pH to pH=8.05 of system.Then by system be placed in sun-drenched place allow expose to the weather 95h (temperature be 5~45
DEG C, wind speed is 4~5m/s) after, precipitation is filtered and washed, is dried to get sample.In the time of this 95h, added every 6 hours
The NaOH solution for entering a 0.0115mol/L, the amount being added every time are:The pH value for first measuring current arrangements, is then added NaOH,
So that pH value increase by 0.05 unit, for example, measure at this time system pH be 7.30, then be added alkali when be added to system always
PH value terminates when being 7.35.
The layered double hydroxide LDH-Cl that the present embodiment is prepared2-I2The draw ratio of whisker is 15~25:1,
Good dispersion, whisker good crystalline, XRD diffraction patterns have the diffractive features of LDH.Therefore, it is the whisker with LDH structures.
Comparative example 1
This comparative example provides a kind of layered double hydroxide LDH-Cl2-I2Preparation method, remove in the preparation method
MgI is prepared in S12·8H2Outside a concentration of 1.6mol/L of O solution, remaining step and operation consistent, this method with embodiment 1
It cannot get whisker, scanning electron microscope (SEM) photograph is as shown in Figure 3:Sample does not have crystal whisker-shaped as seen from Figure 3.
Comparative example 2
This comparative example provides a kind of layered double hydroxide LDH-Cl2-I2Preparation method, remove in the preparation method
AlCl is prepared in S13·6H2Outside a concentration of 0.4mol/L of O solution, remaining step and operation consistent, this method with embodiment 1
It cannot get whisker.
Comparative example 3
This comparative example provides a kind of layered double hydroxide LDH-Cl2-I2Preparation method, remove in the preparation method
The pH that NaOH solution is added to system in S2 is outside 10.0, remaining step is consistent with embodiment 1 with operation, and this method obtains not
To whisker.
Comparative example 4
This comparative example provides a kind of layered double hydroxide LDH-Cl2-I2Preparation method, remove in the preparation method
It is added outside a concentration of 0.5mol/L of NaOH solution in S2, remaining step is consistent with embodiment 1 with operation, and this method obtains not
To whisker.
Comparative example 5
This comparative example provides a kind of layered double hydroxide LDH-Cl2-I2Preparation method, remove in the preparation method
System is placed in outside 60 DEG C in S2, remaining step is consistent with embodiment 1 with operation, and this method cannot get whisker.
Claims (10)
1. a kind of layered double hydroxide LDH-Cl2-I2Whisker, which is characterized in that the chemical formula of the whisker is Mg6Al2
(OH)14Cl2I2·4H2O;The whisker passes through metal cation Mg2+And Al3+With anion Cl-、I-And OH-React to obtain precipitation
Evaporable water obtains afterwards.
2. the layered double-metal hydroxide LDH-Cl of claim 12-I2The preparation method of whisker, which is characterized in that described
Preparation method includes the following steps:
S1:Prepare MgI2And AlCl3Mixed solution, being adjusted to pH with the NaOH of 0.0085 ~ 0.0115mol/L or KOH solution is
7.45~7.55;Mg in the mixed solution2+A concentration of 2.1 ~ 2.7mol/L, Al3+A concentration of 0.65 ~ 0.95mol/L;
S2:After into mixed solution, 0.0085 ~ 0.0115 mol/L NaOH of addition or KOH solution are 7.95 ~ 8.05 to pH, instead
Precipitation should be generated;
S3:Precipitation obtained by S2 is placed at 5 ~ 45 DEG C evaporable water to get layered double-metal hydroxide LDH-Cl2-I2It is brilliant
Palpus.
3. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
It is 7.5 that pH is adjusted in S1.
4. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
Mg in S1 mixed solutions2+A concentration of 2.4mol/L;Al in S1 mixed solutions3+A concentration of 0.8mol/L.
5. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
A concentration of 0.01 mol/L of NaOH described in S2 or KOH solution.
6. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
Be added in S2 NaOH or KOH solution to pH be 8.00.
7. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
The reaction time of S2 is 95 ~ 101h.
8. layered double hydroxide LDH-Cl according to claim 72-I2The preparation method of whisker, which is characterized in that
The pH of mixed solution is adjusted by adding NaOH or KOH solution per 6h in S2, adds the pH before and after NaOH or KOH solution every time
Changing value be not more than 0.05.
9. layered double hydroxide LDH-Cl according to claim 22-I2The preparation method of whisker, which is characterized in that
Further including wind step in S3 makes moisture evaporation, and the wind speed of the wind is 4 ~ 5m/s.
10. the layered double-metal hydroxide LDH-Cl of claim 12-I2Whisker is preparing toughened and reinforced material, catalysis material
Application in material, fire proofing or sorbing material.
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Application publication date: 20180911 |