CN100550213C - A kind of preparation method of nano-conducting attapulgite material - Google Patents
A kind of preparation method of nano-conducting attapulgite material Download PDFInfo
- Publication number
- CN100550213C CN100550213C CNB2006101616815A CN200610161681A CN100550213C CN 100550213 C CN100550213 C CN 100550213C CN B2006101616815 A CNB2006101616815 A CN B2006101616815A CN 200610161681 A CN200610161681 A CN 200610161681A CN 100550213 C CN100550213 C CN 100550213C
- Authority
- CN
- China
- Prior art keywords
- attapulgite
- nano
- preparation
- conducting
- heat treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Non-Insulated Conductors (AREA)
- Powder Metallurgy (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of nano-conducting attapulgite material, it is brilliant that this preparation method at first is dispersed into recessed native aggregation the nano concave earth rod, nano concave earth rod crystalline substance is a nucleome then, adopt the chemical coprecipitation technology at the brilliant coated with uniform one deck conductive compound presoma of nano concave earth rod, mixing by high temperature at last forms 1-dimention nano conducting attapulgite new material.The thermal stability of nano-attapulgite is lower than artificial synthetic fibrous nucleome material, cause in the past method for coating can't make conductive layer evenly continuous and firm attached to the nano-attapulgite surface, primary drying and the heat treatment thermal stability and the surface activity that have improved nano-attapulgite nucleome of the present invention before coating makes the conductive compound presoma evenly be coated on the nano-attapulgite surface on the one hand; Guaranteed that on the other hand conductive coating can not come off in redrying and heat treatment process.Low, the preparation method of nano-conducting attapulgite material production cost of preparation is simple, conduct electricity very well.
Description
Technical field
The present invention relates to the inorganic functional material technical field, specifically, relate to a kind of preparation method of nano-conducting attapulgite material.
Background technology
At present, Chang Yong conductive powder body comprises that metal is that powder, carbon are powder.These two kinds of conductive powder bodies all have certain defective and are restricted when using.Though various metal-powder conductivity are strong, except that silver powder, the easy oxidations of powder such as aluminium, nickel, copper, corrosion-resistant, and the silver powder price is higher.In addition, metal dust is generally than the great caking that easily sinks to the bottom, and is therefore dispersed bad.Though carbon series conductive powder conductivity is better, stability is also good, difficult evenly dispersion, and especially the goods color is black and is not liked by people.Therefore, press for the conductive powder body of exploitation look shallow, conductivity and good stability.
Inorganic light-colored conductive powder body mainly contains two classes: a class is the cladded type electric conducting material, is being nucleome with mica powder, titanium dioxide, zinc oxide, barite etc., and coating layer is the conductive layer that tin ash doping Sb, In, P, F etc. form.To coat the type of tin ash doping Sb, the production cost of cladded type electric conducting material is relatively low in the industrialization product, but specific insulation is higher.Another kind of is doping type electric conductive oxidation powder, as conduction tin ash and conductive zinc oxide etc., is to form defective solid solution by oxide being carried out the high temperature doping, and the production cost of doping type electric conductive oxidation powder is higher relatively, but specific insulation is low.
At present, the key issue that limits inorganic light-colored conductive powder body development is that addition is bigger, and this is because will make the material that adds conductive powder body have conductivity, must be in contact with one another between the conducting particles, or the distance between the particle is little of producing quantum tunneling effect.Generally speaking, make the sheet resistance of material drop to 10
8Below Ω/, the addition of light-colored conductive powder is greater than 25% (wt%), and what have will reach more than 40%, and this not only can increase user's cost greatly, and can reduce the mechanical property of macromolecular material.Therefore, keeping under the constant situation of antistatic effect, the addition that how to reduce the light-colored conductive powder is a problem demanding prompt solution.At this problem, proposed some in the document and improved one's methods: Japanese Ishihara Sangyo Kaisha Ltd. has developed fibrous conductive titanium oxide (U.S. Pat 4880703, US 5320782), fibrous conductive tin oxide (U.S. Pat 5575957) and dendroid conductive titanium oxide (U.S. Pat 6103303).Mitsui Mining ﹠amp; Smelting Co.Ltd has developed fibrous conductive zinc oxide (U.S. Pat 5171364).Sumitomo Chemical Co.Ltd has developed fibrous conduction potassium titanate (U.S. Pat 4933109).Reach same sheet resistance, required fibrous conductive powder body than the graininess conductive powder body lack many because addition is less, can adopt fibrous conductive powder body to make transparent conducting Composite material or transparent conducting coating.In addition, effect such as that the use of fibrous conductive powder body not only can be played is antistatic, INFRARED ABSORPTION, but also can play enhancing, toughness reinforcing effect to the macromolecular material of coating, plastics, rubber, chemical fibre.At present, the preparation of fibrous inorganic conductive material is to be nucleome with artificial synthetic fibrous material, then fibrous nucleome is carried out surface and coats, again by the high temperature formation conductive layer that mixes.Proposing a kind of as Chinese patent CN 1232575C is raw material with six potassium titanates and tin antimonic salt, prepares the method for conductive whiskers with urea for the homogeneous precipitation agent.But the process route of artificial synthetic fibers shape nucleome material is long, and the production cost height causes the on the high side of the fibrous inorganic conductive material for preparing on this basis, has limited extensive use.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano-conducting attapulgite material, common recessed soil is carried out nanometer and functionalization, develop a kind of nano concave earth new material, reduce the production cost of fibrous inorganic conductive material, expand the use field of recessed soil with conducting function.
Technical solution of the present invention is: this preparation method at first is dispersed into the nano-attapulgite crystalline substance with recessed native aggregation, be nucleome with the nano-attapulgite crystalline substance then, adopt the chemical coprecipitation technology at the brilliant coated with uniform one deck of nano-attapulgite conductive compound presoma, mixing by high temperature at last forms 1-dimention nano conducting attapulgite new material.
Preparation method of the present invention comprises following processing step:
(1), natural attapulgite is purified and is disperseed: natural attapulgite mineral are added in the deionized water that is dissolved with dispersant be mixed with the suspension that contains attapulgite 10～120g/L, disperseing the mass ratio of dosage and attapulgite mineral is 1%～8%, mechanical agitation or ultrasonic dispersion 1-5h, leave standstill 5～100h, leave standstill gained upper strata suspension and promptly get the nano-attapulgite dispersion liquid;
(2), primary drying and heat treatment: with nano-attapulgite dispersion liquid spray drying, then at 420～600 ℃ of heat treatment 1～8.0h;
(3) nano-attapulgite surface active and ultrasonic dispersion treatment: primary drying and heat treatment gained nano-attapulgite are placed 1.0～2.0molL
-1Acid solution in carry out surface active, 0～100 ℃ of surface active temperature, surface active time 〉=1h, the ultrasonic or high speed machine dispersion treatment 0.5-5.0h of the acid slurries of the nano-attapulgite of gained behind the surface active;
(4), the nano-attapulgite surface coats: the nano-attapulgite slurry pH value after surface active and the ultrasonic dispersion treatment is adjusted to 1.0～2.5, adjustment to 60～90 ℃, under stirring condition, drip the hydrochloric acid mixed solution and the aqueous slkali of tin antimonic salt simultaneously, it is constant substantially to keep the pH value, and inorganic coating and attapulgite mass ratio are 80%～300%;
(5), Separation of Solid and Liquid and washing: the nano-attapulgite suspension after the surface coated carries out Separation of Solid and Liquid and washing, with deionized water wash to filtrate conductivity≤200 μ S/cm;
(6), redrying and heat treatment: with nano-attapulgite filtration cakes torrefaction, the pulverizing of washes clean, then at 500～700 ℃ of following heat treatment 1～4h.
Described natural attapulgite purify and dispersion steps in dispersant be a kind of in calgon, sodium pyrophosphate, sodium phosphate trimer, Sodium Polyacrylate, the ammonium polyacrylate, two kinds or multiple.
Acid in described nano-attapulgite surface active and the ultrasonic dispersion treatment step is sulfuric acid, nitric acid, hydrochloric acid, perchloric acid, and wherein the hydrochloric acid surface-activation effect is best.
The tin antimonic salt is butter of tin and trichloride antimony in the surperficial encapsulation steps of described nano-attapulgite, and the mass ratio of butter of tin and trichloride antimony is m (SnCl
45H
2O)/m (SbCl
3) be 5～30, optimum quality ratio is 8～20.
The present invention has the following advantages: 1. the thermal stability of nano-attapulgite is lower than artificial synthetic fibrous nucleome material, cause in the past method for coating can't make conductive layer evenly continuous and firm attached to the nano-attapulgite surface, primary drying before coating and heat treatment have improved the thermal stability and the surface activity of nano-attapulgite nucleome, make the conductive compound presoma evenly be coated on the nano-attapulgite surface on the one hand; Guaranteed that on the other hand conductive coating can not come off in redrying and heat treatment process.2. the nano-conducting attapulgite material production cost of the present invention preparation is low, the preparation method simple, conduct electricity very well.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment.
The mensuration of powder specific insulation of the present invention: in the polyacrylate glass tube of a band scale, put into 10.0g conductive nano titanium dioxide powder, pressure with 1MPa is pressed in conductive powder body between the two metal sheets, measure resistance between two metal sheets with universal meter, the resistivity that is calculated as follows conductive powder body according to the thickness and the sectional area of powder layer.
R
sp＝R×A/L
In the formula: R
SpBe specific insulation (Ω cm) that R is actual measurement resistance (Ω), A is the internal diameter sectional area (cm of glass tube
2), L is the height (cm) of conductive powder body layer.
Embodiment 1: natural attapulgite mineral are added in the deionized water that the mass ratio that is dissolved with attapulgite is 1% calgon, be mixed with the suspension that contains attapulgite 10g/L, ultrasonic dispersion 1h leaves standstill 5h; With gained nano-attapulgite dispersion liquid spray drying, then at 420 ℃ of following heat treatment 8.0h; Nano-attapulgite after primary drying and the heat treatment is placed 1.0molL
-1Hydrochloric acid solution in, under 0 ℃, carry out surface active 24h, ultrasonic then dispersion 0.5h; The pH value of the nano-attapulgite slurries after surface active and the ultrasonic dispersion treatment is adjusted to 1.0, is warming up to 90 ℃, under stirring condition, drip 0.4molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=5 drip 2.0molL simultaneously
-1Sodium hydroxide solution, constant substantially with the pH value that keeps solution, dropping SnO in the 3h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 80%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 10h under 110 ℃, pulverizes 500 ℃ of following heat treatment 4h.The specific insulation of gained powder is 1500 Ω cm.
Embodiment 2: it is in 8% the ammonium polyacrylate deionized water that natural attapulgite mineral are added the mass ratio that is dissolved with attapulgite, is mixed with the suspension that contains attapulgite 120g/L, with mulser high speed dispersion 5h, leaves standstill 100h; With gained nano-attapulgite dispersion liquid spray drying, then at 600 ℃ of following heat treatment 1h; Nano-attapulgite after primary drying and the heat treatment places 2.0molL
-1Hydrochloric acid solution in, under 100 ℃, carry out surface active 1h, disperse 5h with the mulser high speed machine then; The pH value of the nano-attapulgite slurries after surface active and the mechanical dispersion processing is adjusted to 2.5, and temperature transfers to 60 ℃, under stirring condition, drips 0.4molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=30 drip 2.0molL simultaneously
-1Potassium hydroxide solution, constant substantially with the pH value that keeps solution, dropping SnO in the 10h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 300%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 24h under 95 ℃, pulverizes 700 ℃ of following heat treatment 1h.The specific insulation of gained powder is 100 Ω cm.
Embodiment 3: it is in 3% the sodium pyrophosphate deionized water that natural attapulgite mineral are added the mass ratio that is dissolved with attapulgite, is mixed with the suspension that contains attapulgite 80g/L, with mulser high speed dispersion 3h, leaves standstill 30h; With gained nano-attapulgite dispersion liquid spray drying, then at 450 ℃ of following heat treatment 2h; Nano-attapulgite after primary drying and the heat treatment places 1.6molL
-1Hydrochloric acid solution in, under 70 ℃, carry out surface active 2h, ultrasonic then dispersion 1h; The pH value of the nano-attapulgite slurries after surface active and the ultrasonic dispersion treatment is adjusted to 1.5, and temperature transfers to 75 ℃, under stirring condition, drips 0.3molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=10 drip 2.0molL simultaneously
-1Ammonia spirit, constant substantially with the pH value that keeps solution, dropping SnO in the 8h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 200%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 5h under 150 ℃, pulverizes 550 ℃ of following heat treatment 2h.The specific insulation of gained powder is 10 Ω cm.
Embodiment 4: among the embodiment 4, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=5, other operation is all identical with embodiment 3.The specific insulation of gained powder is 72 Ω cm.
Embodiment 5: among the embodiment 5, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=8, other operation is all identical with embodiment 3.The specific insulation of gained powder is 15 Ω cm.
Embodiment 6: among the embodiment 6, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=15, other operation is all identical with embodiment 3.The specific insulation of gained powder is 11 Ω cm.
Embodiment 7: among the embodiment 7, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=20, other operation is all identical with embodiment 3.The specific insulation of gained powder is 21 Ω cm.
Embodiment 8: among the embodiment 8, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=25, other operation is all identical with embodiment 3.The specific insulation of gained powder is 110cm.
Embodiment 9: among the embodiment 9, remove m (SnCl
45H
2O)/m (SbCl
3Outside)=30, other operation is all identical with embodiment 3.The specific insulation of gained powder is 340 Ω cm.
Embodiment 10: among the embodiment 10, remove and change surfactant into 1.6molL
-1Nitric acid liquid outside, other operation is all identical with embodiment 3.The specific insulation of gained powder is 90 Ω cm.
Embodiment 10: among the embodiment 10, remove and change surfactant into 1.6molL
-1Perchloric acid liquid outside, other operation is all identical with embodiment 3.The specific insulation of gained powder is 80 Ω cm.
Embodiment 11: among the embodiment 10, remove and change surfactant into 0.8molL
-1Sulfuric acid liquid outside, other operation is all identical with embodiment 3.The specific insulation of gained powder is 115 Ω cm.
Embodiment 12: natural attapulgite mineral are added in the deionized water that the mass ratio that is dissolved with attapulgite is 3% Sodium Polyacrylate, be mixed with the suspension that contains attapulgite 30g/L, with mulser high speed dispersion 1h, leave standstill 10h; With gained nano-attapulgite dispersion liquid spray drying, then at 440 ℃ of following heat treatment 4.0h; Nano-attapulgite is placed 1.0molL
-1Sulfuric acid liquid in, under 50 ℃, carry out surface active 12h, ultrasonic then dispersion 0.5h; The pH value of the nano-attapulgite slurries after surface active and the ultrasonic dispersion treatment is adjusted to 1.5, is warming up to 80 ℃, under stirring condition, drips 0.2molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=12 drip 1.0molL simultaneously
-1Sodium carbonate liquor, constant substantially with the pH value that keeps solution, dropping is with SnO in the 5h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 150%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 5h under 150 ℃, pulverizes 550 ℃ of following heat treatment 2h.The specific insulation of gained powder is 50 Ω cm.
Embodiment 13: natural attapulgite mineral are added in the deionized water that the mass ratio that is dissolved with attapulgite is 5% sodium phosphate trimer, be mixed with the suspension that contains attapulgite 50g/L, with the ultrasonic dispersion of ultrasonic disperser 2h, leave standstill 24h; With gained nano-attapulgite dispersion liquid spray drying, then at 460 ℃ of following heat treatment 2h; Nano-attapulgite is placed 1.5molL
-1Hydrochloric acid solution in, under 20 ℃, carry out surface active 24h, ultrasonic then dispersion 1.0h; Nano-attapulgite pH value of slurry after surface active and the ultrasonic dispersion treatment is adjusted to 1.5, is warming up to 80 ℃, under stirring condition, drips 0.5molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=15 drip 2.0molL simultaneously
-1Ammonia spirit, constant substantially with the pH value that keeps solution, dropping is with SnO in the 6h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 200%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 10h under 110 ℃, pulverizes 600 ℃ of following heat treatment 2h.The specific insulation of gained powder is 20 Ω cm.
Embodiment 14: natural attapulgite mineral are added in the deionized water of Sodium Polyacrylate that the mass ratio that is dissolved with attapulgite is 1% sodium pyrophosphate and 2%, be mixed with the suspension that contains attapulgite 80g/L, with mulser high speed dispersion 2h, ultrasonic dispersion 1h leaves standstill 50h; With gained nano-attapulgite dispersion liquid spray drying, then at 480 ℃ of following heat treatment 4.0h; Nano-attapulgite is placed 2.0molL
-1Hydrochloric acid solution in, under 70 ℃, carry out surface active 8h, use mulser high speed dispersion 5h then; Nano-attapulgite pH value of slurry after surface active and the dispersion treatment is adjusted to 2.0, is warming up to 90 ℃, under stirring condition, drips 0.6molL
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=20 drip 3.0molL simultaneously
-1Potassium hydroxide solution, constant substantially with the pH value that keeps solution, dropping is with SnO in the 6h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 250%, after dripping off, and slaking 0.5h; Filter, nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 15h under 100 ℃, pulverizes 650 ℃ of following heat treatment 3h.The specific insulation of gained powder is 10 Ω cm.
Embodiment 15: natural attapulgite mineral are added in the deionized water that the mass ratio that is dissolved with attapulgite is 1% sodium phosphate trimer, 2% sodium pyrophosphate, 2% ammonium polyacrylate, be mixed with the suspension that contains attapulgite 100g/L, with mulser high speed dispersion 2h, leave standstill 100h; With gained nano-attapulgite dispersion liquid spray drying, then at 500 ℃ of following heat treatment 7.0h; Nano-attapulgite is placed 2.0molL
-1Hydrochloric acid solution in, under 70 ℃, carry out surface active 6h, ultrasonic then dispersion 1h; Nano-attapulgite pH value of slurry after surface active and the ultrasonic dispersion treatment is adjusted to 1.7, is warming up to 80 ℃, under stirring condition, and the 0.3molL of dropping
-1The hydrochloric acid mixed solution of butter of tin and trichloride antimony, m (SnCl
45H
2O)/m (SbCl
3)=17 drip 2.0molL simultaneously
-1Sodium hydroxide solution, constant substantially with the pH value that keeps solution, dropping is with SnO in the 5h
2Meter accounts for the tin antimony mixed liquor of attapulgite quality 300%, after dripping off, and slaking 0.5h; Nano-attapulgite suspension is carried out Separation of Solid and Liquid, use deionized water wash, wash conductivity to filtrate less than 200 μ s/cm; The nano-attapulgite filter cake that washing finishes is dry 8h under 120 ℃, pulverizes 700 ℃ of following heat treatment 2h.The specific insulation of gained powder is 10 Ω cm.
Comparative example 1～15:
In comparative example 1～15, primary drying among the embodiment 1～15 and heat treated step to be saved, other operation is all identical with embodiment 1～15.The specific insulation of gained powder is for all greater than 10000 Ω cm.
Claims (4)
1. the preparation method of a nano-conducting attapulgite material, it is brilliant that this preparation method at first is dispersed into recessed native aggregation the nano concave earth rod, nano concave earth rod crystalline substance is a nucleome then, adopt the film soverlay technique at the brilliant coated with uniform one deck conductive compound presoma of nano concave earth rod, mix by high temperature at last and form 1-dimention nano conducting attapulgite new material, comprise following processing step:
(1), natural attapulgite is purified and is disperseed: natural attapulgite mineral are added in the deionized water that is dissolved with dispersant be mixed with the suspension that contains attapulgite 10～120g/L, disperseing the mass ratio of dosage and attapulgite mineral is 1%～8%, mechanical agitation or ultrasonic dispersion 1-5h, leave standstill 5～100h, leave standstill gained upper strata suspension and be the nano-attapulgite dispersion liquid;
(2), primary drying and heat treatment: with nano-attapulgite dispersion liquid spray drying, then at 420～600 ℃ of heat treatment 1～8.0h;
(3), nano-attapulgite surface active and ultrasonic dispersion treatment: primary drying and heat treatment gained nano-attapulgite are placed 1.0～2.0molL
-1Acid solution in carry out surface active, 0～100 ℃ of surface active temperature, surface active time 〉=1h, the ultrasonic or high speed machine dispersion treatment 0.5-5.0h of the acid slurries of the nano-attapulgite of gained behind the surface active;
(4), the nano-attapulgite surface coats: the nano-attapulgite slurry pH value after surface active and the ultrasonic dispersion treatment is adjusted to 1.0～2.5, adjustment to 60～90 ℃, under stirring condition, drip the hydrochloric acid mixed solution and the aqueous slkali of tin antimonic salt simultaneously, it is constant substantially to keep the pH value, and inorganic coating is with SnO
2Meter is 80%～300% with the attapulgite mass ratio;
(5), Separation of Solid and Liquid and washing: the nano-attapulgite suspension after the surface coated carries out Separation of Solid and Liquid and washing, with deionized water wash to filtrate conductivity≤200 μ S/cm;
(6), redrying and heat treatment: with nano-attapulgite filtration cakes torrefaction, the pulverizing of washes clean, then at 500～700 ℃ of following heat treatment 1～4h.
2. the preparation method of a kind of nano-conducting attapulgite material according to claim 1 is characterized in that: described natural attapulgite purify and dispersion steps in dispersant be a kind of in calgon, sodium pyrophosphate, sodium phosphate trimer, Sodium Polyacrylate, the ammonium polyacrylate, two kinds or multiple.
3. the preparation method of a kind of nano-conducting attapulgite material according to claim 2, it is characterized in that: the acid in described nano-attapulgite surface active and the ultrasonic dispersion treatment step is sulfuric acid, nitric acid, hydrochloric acid, perchloric acid.
4. the preparation method of a kind of nano-conducting attapulgite material according to claim 2, it is characterized in that: the tin antimonic salt is SnCl in the surperficial encapsulation steps of described nano-attapulgite
45H
2O and SbCl
3, SnCl
45H
2O and SbCl
3Mass ratio be 5～30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101616815A CN100550213C (en) | 2006-12-31 | 2006-12-31 | A kind of preparation method of nano-conducting attapulgite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101616815A CN100550213C (en) | 2006-12-31 | 2006-12-31 | A kind of preparation method of nano-conducting attapulgite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101000809A CN101000809A (en) | 2007-07-18 |
| CN100550213C true CN100550213C (en) | 2009-10-14 |
Family
ID=38692728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101616815A Expired - Fee Related CN100550213C (en) | 2006-12-31 | 2006-12-31 | A kind of preparation method of nano-conducting attapulgite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100550213C (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812209B (en) * | 2010-04-01 | 2011-06-29 | 江苏工业学院 | Method for preparing nanometer attapulgite/polyvinyl acetate composite emulsion |
| CN101805605A (en) * | 2010-04-12 | 2010-08-18 | 东南大学 | Attapulgite clay quantum dot nano-composite fluorescent material and preparation method thereof |
| CN101935489A (en) * | 2010-08-24 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Concave-convex rod conductive coating and preparation method thereof |
| CN102502678A (en) * | 2011-09-21 | 2012-06-20 | 镇江忆诺唯记忆合金有限公司 | Preparation method of nanometer TiO2-ATP (Adenosine Triphosphate) powder material |
| CN102977491B (en) * | 2012-11-22 | 2015-02-25 | 芜湖跃飞新型吸音材料股份有限公司 | Nano attapulgite modified composite sound absorbing material and preparation method thereof |
| CN103553062A (en) * | 2013-10-30 | 2014-02-05 | 盐城工学院 | Modified ATP (attapulgite) material as well as preparation method and application thereof |
| CN104124002B (en) * | 2014-07-18 | 2017-12-05 | 江苏启弘新材料科技有限公司 | A kind of preparation method of light-colored conductive attapulgite powder |
| CN105238100A (en) * | 2015-10-23 | 2016-01-13 | 渤海大学 | Method for preparing light-colored conductive titanium dioxide |
| CN107500304B (en) * | 2017-08-30 | 2020-02-04 | 饶伟锋 | Preparation method of light-color electrically-insulated laser-activated metallizable powder |
| CN111013559B (en) * | 2019-12-25 | 2023-07-18 | 常州纳欧新材料科技有限公司 | Mixed crystal type ternary structure composite material, preparation method thereof and application thereof in photocatalytic denitrification |
| CN111849214A (en) * | 2020-08-21 | 2020-10-30 | 扬州大学 | Efficient preparation of core-shell ATO @ TiO2Method for conducting whiskers |
| CN112391076B (en) * | 2020-10-29 | 2022-03-22 | 淮阴工学院 | Attapulgite composite nano material and preparation method and application thereof |
-
2006
- 2006-12-31 CN CNB2006101616815A patent/CN100550213C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101000809A (en) | 2007-07-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100550213C (en) | A kind of preparation method of nano-conducting attapulgite material | |
| CN105271389B (en) | A kind of preparation method of conductive titanium dioxide powder | |
| CN101333345B (en) | Method for preparing nanometer titanium dioxide/attapulgite composite material | |
| CN102148351B (en) | Preparation method for electrode material of lithium battery | |
| DE69033486T2 (en) | Battery and carbon fiber bundle for making the same | |
| CN101747625B (en) | Attapulgite/ titanium dioxide/silicon dioxide/polyaniline nanometer conductive composite material and preparation method thereof | |
| CN104327574B (en) | Micro/nano Cu2O/ZnO composite material, preparation method and application thereof | |
| CN105238100A (en) | Method for preparing light-colored conductive titanium dioxide | |
| CN100378870C (en) | Process for preparing nano-oxide conducting powder | |
| CN101182052B (en) | Treatment of alkaline black liquor by bubble liquid membrane bittern method | |
| CN101708555B (en) | Method for preparing flake silver powder | |
| CN101423673B (en) | Method for improving brightness of attapulgite | |
| CN106497148B (en) | A kind of high conductivity nano biological carbon black and its preparation method and application | |
| CN100360424C (en) | Method for preparing nano antimony-doped tin dioxide powder | |
| CN102616791B (en) | Method for preparing white carbon black from diatomite in situ | |
| CN102776524B (en) | The preparation method of nanometer selenium | |
| CN106187161A (en) | Heat insulation conductive material of light colour flaky and preparation method thereof | |
| CN102249293A (en) | Method for preparing pyrophillite-based antimony-doped tin oxide compound conductive powder | |
| CN1132885C (en) | Process for preparing conducting light colour flaky pigment | |
| CN107188225B (en) | A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof | |
| CN105932271A (en) | Preparation method of cobaltosic oxide/stannic oxide composite nanomaterial | |
| CN105417575A (en) | Preparation method of monodisperse tin dioxide quantum dot hydrosol | |
| CN103756370A (en) | Electro-conductive pearlescent pigment | |
| CN101805017A (en) | Preparation method of rutile type titanium dioxide nano particle | |
| CN102838159B (en) | Method for synthesizing nano-zinc oxide by micro-emulsion carbon black adsorption precipitation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091014 Termination date: 20141231 |
|
| EXPY | Termination of patent right or utility model |