CN107961763A - The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia - Google Patents
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method for adsorbing carbon nanotubes/LDHs composite materials of metal ion in ultra-pure ammonia, by the way that carbon nanotubes and anion surfactant or anionic polyelectrolyte are carried out reaction modification under hydrothermal condition, so that carbon nano tube surface carries negative electrical charge, so as to be combined with each other to form composite material with LDHs using the principle of the replaceable insertion of LDHs interlayer anions, the beneficial effects of the invention are as follows：By negatively charged carbon nanotubes intercalation after anion modified into LDHs interlayers, both the suction-operated of carbon nano tube surface functional group had been make use of, solve the problems, such as that carbon nanotubes cannot be separately as metal ion adsorbent in ultra-pure ammonia again, carbon nanotubes and the electrostatic interaction of LDHs laminates greatly strengthen suction-operated of the carbon nanotubes to metal ion in itself again at the same time, play the role of being used alone considerably beyond carbon nanotubes and LDHs.
Description
Technical field
The application is to be directed to Application No. 201610195223.7, and the applying date is on March 31st, 2016, entitled " a kind of
The division Shen of the application for a patent for invention of the preparation method of carbon nanotubes/LDHs composite materials of metal ion in absorption ultra-pure ammonia "
Please.
The present invention relates to a kind of preparation method of composite material, more particularly to a kind of carbon nanotubes and LDHs composite materials
Preparation method, belongs to technical field of composite materials.
Background technology
In recent years, the LED technology in China and related industry are grown rapidly, with the hair of the photoelectronic industries such as LED
Exhibition, market proposes requirements at the higher level to the purity of electronic gas, so greatly having promoted upstream key supplementary material ultra-pure ammonia
Purification research.
7N electronic grade ultrapure ammonias are a kind of very important photoelectron materials, and MOCVD technologies prepare the weight of GaN
Basic material is wanted, the gallium nitride used in LED productions is semi-conducting material, so in process of production, it is necessary to in raw material
Metal ion is strictly controlled, and still, mainly utilizes ammonia to the purifying process of metal ion in ultra-pure ammonia both at home and abroad at present
The physicochemical property of gas is purified step by step using multistep, including vaporize, condense, adsorbing, rectifying, terminal purifying, freezing etc. technology purification
Ammonia, the purifying process of these ammonia is usually to moisture and H2、O2、N2、CH4, the light component impurity such as CO have preferable effect, it is and right
The effect that metal ion removes is undesirable.
Carbon nanotubes has unique structure and unusual property, from carbon nanotubes by since finding first, its performance and
Using all widely being studied, carbon nanotubes is hollow and two end seals crimped by the hexagonal mesh of similar graphite
The multilayer tubular thing closed, carbon nanotube diameter is between several nanometers to several tens of nanometers, and length is up to a few micrometers, its synusia spacing one
As be 0.34nm, since it is with great specific surface area and chemical stability, and unique electronic structure, vestibule structure and
Absorption property, excellent electronic conductivity, special vestibule space multistory selectivity, causes it to be produced for reaction species and reaction
Thing has special absorption property, and carbon nanotubes can pass through electrostatic attraction, adsorption precipitation and metal ion and carbon nanotubes
The chemical action of surface functional group carry out adsorbing metal ions, but carbon nanotubes cannot be placed directly in ultra-pure ammonia, so
Although metal ion can be removed, carbon nanotubes cannot can cause ultra-pure ammonia new with ultrapure ammonia separation after removal
Pollution, works so carbon nanotubes will be attached on other materials.
Layered double hydroxide (LDHs) is a kind of anion lamellar compound, also known as hydrotalcite, and LDHs is by layer
Between anion and the accumulation of positively charged laminate form, there is the structure that can be embedded in anion, the structure such as sandwich of LDHs
Shape, both sides are made of the metal ion positive charge piece of divalence and trivalent, and centre is anion and hydrone, the main layer board of LDHs
With the particularity of the Nomenclature Composition and Structure of Complexes of interlayer object, the numerous special performances of LDHs are imparted, the anion of LDHs interlayers can be with
Anion with various specific functions swaps, so as to synthesize the intercalation configuration material with different performance.
The content of the invention
The present invention is for insufficient existing for adsorption of metal ions technology in existing ultra-pure ammonia, there is provided in one kind absorption ultra-pure ammonia
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia, it is characterised in that
Include the following steps：
1) preparation of LDHs：Soluble magnesium salts and aluminium salt are placed in dissolving in deionized water are configured to total concentration and be
The solution A of 0.5mol/L, Mg:Al=1:2, aqueous slkali B is added dropwise in solution A under constant agitation, in this process
It is middle holding solution ph 9~10, aqueous slkali B continue after being added dropwise stirring ageing 3~5 it is small when, filtering, wash repeatedly into
Property, products obtained therefrom is placed in when 6~10 is small in 80~100 DEG C of baking oven colloidal sol is made；
2) acidifying of carbon nanotubes：The aqueous solution of oxidizing acid is added into carbon nanotubes, 110~130 DEG C of conditions are next time
When stream 2~5 is small, centrifuges, washed with clear water to neutrality, the carbon nanotubes being acidified；
3) negatively charged carbon nanotubes is prepared：The carbon nanotubes of the acidifying of gained in step 2) is added to anion to gather
In the aqueous solution of electrolyte or anion surfactant, when ultrasonication 1~3 is small, stirred after in 50~70 DEG C of water-baths
When reaction 4~10 is small under the conditions of mixing, the concentration of aqueous solution of the anionic polyelectrolyte or anion surfactant for 1~
10g/L, the carbon nanotubes are 1 with the weight ratio of anionic polyelectrolyte or anion surfactant：(0.01~0.1),
Centrifuged after having reacted and remove unreacted anionic polyelectrolyte or anion surfactant, obtained surface and carry negative electricity
The carbon nanotubes of lotus；
4) carbon nanotubes/LDHs compounds are prepared：The carbon nanotubes of gained in step 3) is added to obtained by step 1)
In colloidal sol, the weight ratio of carbon nanotubes and colloidal sol is 1：(20~30), after the mixture of the two is placed in 50~70 DEG C of water-baths
Ion-exchange reactions is carried out under stirring condition, when the reaction time 6~8 is small, filtering and washing, dry after completion of the reaction, obtains carbon and receives
Mitron/LDHs compounds.
Further, aluminium salt described in step 1) and magnesium salts are aluminum nitrate and magnesium nitrate, and the aqueous slkali is molten for sodium hydroxide
Liquid.
Further, oxidizing acid described in step 2) refers to the one or more in nitric acid, sulfuric acid, permanganic acid, hypochlorous acid
Mixture.
Further, the anionic polyelectrolyte described in step 3) is kayexalate, in sodium lignin sulfonate
One or more, the anion surfactant are neopelex.
Further, the carbon nanotubes is one kind in single-walled carbon nanotube, multi-walled carbon nanotube.
The beneficial effects of the invention are as follows：
1) negatively charged carbon nanotubes intercalation after anion modified carbon nanotubes table had both been make use of into LDHs interlayers
The suction-operated of face functional group, but solve the problems, such as carbon nanotubes cannot separately as metal ion adsorbent in ultra-pure ammonia,
Carbon nanotubes and the electrostatic interaction of LDHs laminates greatly strengthen suction-operated of the carbon nanotubes to metal ion in itself again at the same time,
Play the role of being used alone considerably beyond carbon nanotubes and LDHs；
2) whole preparation process reaction condition is gentle, easy to operate, it is easy to accomplish.
The compound of gained of the invention can be filled in the drier in ultra-pure ammonia prepurification stage, instead of original common water removal
The molecular sieve of deoxygenation, can also be placed in the transfer pipeline of ultra-pure ammonia as adsorbent.
Embodiment
The principle of the present invention and feature are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Embodiment 1：
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia, including following step
Suddenly：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody
It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to
5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition
System pH is kept 9~10, NaOH solution continue after being added dropwise stirring ageing 3 it is small when, products therefrom is filtered, using going
Ionized water is washed 3 times repeatedly, is placed in the hydrotalcite colloidal sol for being made that solid content is 2wt% when 6 is small in 100 DEG C of thermostatic drying chambers；
2) 20~40nm of diameter of 100g Shenzhen nanometer port Co., Ltd purchase, the multi-wall carbon nano-tube that 1~2 μm of length are weighed
Pipe, adds the nitric acid 500ml of 3mol/L thereto, be heated at 120 DEG C reflux 3 it is small when, be cooled to room temperature, centrifuge, clearly
Water washing is to neutrality, the carbon nanotubes being acidified；
3) the carbon nanotubes 50g for weighing the acidifying of gained in step 2) is added to the polystyrene that 500ml concentration is 6g/L
In sodium sulfonate (abbreviation PSS) aqueous solution, be initially positioned in 20Hz ultrasonic devices ultrasound 2 it is small when, be placed on 60 DEG C of stirred in water bath bars
When reaction 5 is small under part, is centrifuged after having reacted and remove unreacted PSS, obtain the carbon nanotubes that surface carries negative electrical charge；
4) the carbon nanotubes 20g of gained in step 3) is taken to be placed in 400g steps 1) in the colloidal sol of gained, by the mixed of the two
Compound, which is placed under the conditions of 50 DEG C of stirred in water bath, carries out ion-exchange reactions, when reaction 6 is small after filtering and washing, it is dry, obtain carbon and receive
Mitron/LDHs compounds.
Embodiment 2：
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia, including following step
Suddenly：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody
It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to
5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition
System pH is kept 9~10, NaOH solution continue after being added dropwise stirring ageing 3 it is small when, products therefrom is filtered, using going
Ionized water is washed 3 times repeatedly, is placed in the hydrotalcite colloidal sol for being made that solid content is 2wt% when 6 is small in 100 DEG C of thermostatic drying chambers；
2) 20~40nm of diameter of 100g Shenzhen nanometer port Co., Ltd purchase, the multi-wall carbon nano-tube that 1~2 μm of length are weighed
Pipe, adds the sulfuric acid 500ml of 5mol/L thereto, be heated at 130 DEG C reflux 2 it is small when, be cooled to room temperature, centrifuge, clearly
Water washing is to neutrality, the carbon nanotubes being acidified；
3) the carbon nanotubes 50g for weighing the acidifying of gained in step 2) is added to the dodecyl that 500ml concentration is 1g/L
In benzene sulfonate aqueous solution, be initially positioned in 20HZ ultrasonic devices ultrasound 1 it is small when, be placed under the conditions of 70 DEG C of stirred in water bath and react
4 it is small when, centrifuged after having reacted and remove unreacted neopelex, obtain the carbon nanometer that surface carries negative electrical charge
Pipe；
4) the carbon nanotubes 30g of gained in step 3) is taken to be placed in 750g steps 1) in the colloidal sol of gained, by the mixed of the two
Compound, which is placed under the conditions of 60 DEG C of stirred in water bath, carries out ion-exchange reactions, when reaction 8 is small after filtering and washing, it is dry, obtain carbon and receive
Mitron/LDHs compounds.
Embodiment 3：
The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia, including following step
Suddenly：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody
It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to
5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition
System pH is kept 9~10, NaOH solution continue after being added dropwise stirring ageing 3 it is small when, products therefrom is filtered, using going
Ionized water is washed 3 times repeatedly, is placed in the hydrotalcite colloidal sol for being made that solid content is 5wt% when 6 is small in 100 DEG C of thermostatic drying chambers；
2) 20~40nm of diameter of 100g Shenzhen nanometer port Co., Ltd purchase, the single that 1~2 μm of length are weighed
Pipe, adds the permanganic acid 500ml of 3mol/L thereto, be heated at 110 DEG C reflux 5 it is small when, be cooled to room temperature, centrifuge,
Clear water is washed to neutrality, the carbon nanotubes being acidified；
3) the carbon nanotubes 50g for weighing the acidifying of gained in step 2) is added to the sulfomethylated lignin that 500ml concentration is 10g/L
In acid sodium aqueous solution, be initially positioned in 20HZ ultrasonic devices ultrasound 1 it is small when, reaction 10 is small under the conditions of being placed on 50 DEG C of stirred in water bath
When, centrifuged after having reacted and remove unreacted sodium lignin sulfonate, obtain the carbon nanotubes that surface carries negative electrical charge；
4) the carbon nanotubes 20g of gained in step 3) is taken to be placed in 600g steps 1) in the colloidal sol of gained, by the mixed of the two
Compound, which is placed under the conditions of 70 DEG C of stirred in water bath, carries out ion-exchange reactions, when reaction 8 is small after filtering and washing, it is dry, obtain carbon and receive
Mitron/LDHs compounds.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (6)
- A kind of 1. preparation method for adsorbing carbon nanotubes/LDHs composite materials of metal ion in ultra-pure ammonia, it is characterised in that bag Include following steps：1) preparation of LDHs：It is 0.5mol/L that soluble magnesium salts and aluminium salt be placed in deionized water dissolving is configured to total concentration Solution A, Mg:Al=1:2, aqueous slkali B is added dropwise in solution A under constant agitation, keeps molten in the process Liquid pH value 9~10, aqueous slkali B continue after being added dropwise stirring ageing 3~5 it is small when, filtering, wash repeatedly to neutrality, by gained Product is placed in when 6~10 is small in 80~100 DEG C of baking oven and colloidal sol is made；2) acidifying of carbon nanotubes：The aqueous solution of oxidizing acid is added into carbon nanotubes, reflux 2 under the conditions of 110~120 DEG C~ 3 it is small when, centrifuge, washed with clear water to neutrality, the carbon nanotubes being acidified；3) negatively charged carbon nanotubes is prepared：The carbon nanotubes of the acidifying of gained in step 2) is added to anionic polyelectrolyte In the aqueous solution of matter or anion surfactant, when ultrasonication 1~2 is small, after 60~70 DEG C of stirred in water bath bars When reaction 4~5 is small under part, the concentration of aqueous solution of the anionic polyelectrolyte or anion surfactant is 6~10g/L, The carbon nanotubes is 1 with the weight ratio of anionic polyelectrolyte or anion surfactant：(0.06~0.1), it is described Anionic polyelectrolyte is kayexalate, the one or more in sodium lignin sulfonate, and the anionic surface is lived Property agent be neopelex, centrifuged after having reacted and remove unreacted anionic polyelectrolyte or anionic surface Activating agent, obtains the carbon nanotubes that surface carries negative electrical charge；4) carbon nanotubes/LDHs compounds are prepared：The carbon nanotubes of gained in step 3) is added to the colloidal sol obtained by step 1) In, the weight ratio of carbon nanotubes and colloidal sol is 1：(25~30), after the mixture of the two is placed in 60~70 DEG C of stirred in water bath Under the conditions of carry out ion-exchange reactions, when the reaction time 8 is small, filtering and washing after completion of the reaction is dry, obtain carbon nanotubes/ LDHs compounds.
- 2. the preparation side of carbon nanotubes/LDHs composite materials of metal ion in absorption ultra-pure ammonia according to claim 1 Method, it is characterised in that aluminium salt described in step 1) and magnesium salts are aluminum nitrate and magnesium nitrate, and the aqueous slkali is molten for sodium hydroxide Liquid.
- 3. the preparation side of carbon nanotubes/LDHs composite materials of metal ion in absorption ultra-pure ammonia according to claim 1 Method, it is characterised in that oxidizing acid described in step 2) refers to one or more of in nitric acid, sulfuric acid, permanganic acid, hypochlorous acid Mixture.
- 4. the preparation side of carbon nanotubes/LDHs composite materials of metal ion in absorption ultra-pure ammonia according to claim 1 Method, it is characterised in that the carbon nanotubes is single-walled carbon nanotube, one kind in multi-walled carbon nanotube.
- 5. carbon nanotubes/LDHs of metal ion is compound in a kind of absorption ultra-pure ammonia as any one of claim 1-4 The preparation method of material prepares carbon nanotubes/LDHs composite materials of gained.
- A kind of 6. carbon nanotubes/LDHs composite materials metal ion field in ultra-pure ammonia is adsorbed as claimed in claim 5 Using.
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| CN201810000927.3A CN107961763A (en) | 2016-03-31 | 2016-03-31 | The preparation method of the carbon nanotubes of metal ion/LDHs composite materials in a kind of absorption ultra-pure ammonia |
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| CN111559742A (en) * | 2019-12-25 | 2020-08-21 | 江西悦安新材料股份有限公司 | Method for improving stability of carbon nano tube |
| CN112090378A (en) * | 2020-07-29 | 2020-12-18 | 淮阴工学院 | Preparation method of photo-thermal conversion enhanced microcapsule phase change material |
| CN112683871B (en) * | 2021-01-05 | 2021-09-21 | 江苏雨松环境修复研究中心有限公司 | Soil chromium ion content detection method |
| CN113104872B (en) * | 2021-05-24 | 2022-10-21 | 北京化工大学 | Method for preparing organic molecule intercalation hydrotalcite array by one-step method |
| CN113318709A (en) * | 2021-06-04 | 2021-08-31 | 董鹏 | Oil stain adsorbent and preparation method thereof |
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