CN104124002A - Method for preparing light-colored conductive attapulgite powder - Google Patents

Method for preparing light-colored conductive attapulgite powder Download PDF

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Publication number
CN104124002A
CN104124002A CN201410348252.3A CN201410348252A CN104124002A CN 104124002 A CN104124002 A CN 104124002A CN 201410348252 A CN201410348252 A CN 201410348252A CN 104124002 A CN104124002 A CN 104124002A
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solution
attapulgite
light
sncl
colored conductive
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CN104124002B (en
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刘水平
夏清明
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JIANGSU QIHONG NEW MATERIAL TECHNOLOGY Co Ltd
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JIANGSU QIHONG NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a method for preparing light-colored conductive attapulgite powder. A certain quantity of attapulgite is added to a prepared SnCl4 solution; ammonium hydroxide is slowly dropwise added into the SnCl4 solution with the attapulgite, after dropwise adding and then standing for a couple of hours, an attapulgite solution with deposited Sn(OH) 4 seed crystals on the surface is obtained, SnCl4 and SbCl3 are added into a hydrochloric acid in a certain concentration to form a mixed solution, and the mixed solution and the ammonium hydroxide are simultaneously slowly dropwise added into the seed crystal solution during stirring; filtering is performed, obtained solids are cleanly washed by deionized water, an obtained substance is placed in a vacuum drying oven to be dried and then placed in a muffle furnace to be calcined, and corresponding light-colored conductive attapulgite powder can be obtained.

Description

A kind of preparation method of light-colored conductive attapulgite powder
Technical field
The present invention relates to a kind of preparation of light-colored conductive attapulgite, belong to the functional modification technology of nano particle.
Background technology
Along with the raising of living standards of the people with to the requirement of quality of the life, improve, for the demand of antistatic/conductive fabric, constantly expand, traditional dark carbon is that antistatic/conductive fiber can not satisfy the demands, needs exploitation light-colored antistatic/conductive fiber badly.This technological invention, for the preparation of light-colored antistatic/conductive fiber, has proposed a kind of preparation method of novel light-colored conductive attapulgite powder, for the preparation of light-colored antistatic/conductive fiber lays the foundation.
The shape of conductive filler has larger impact for the performance of conductive polymeric composite and the materials of filler.For reducing the consumption of conductive filler, the bar-shaped conductive filler of general selection.Attapulgite is a kind of natural clay with one-dimensional rod-like structure, take attapulgite as core is when its surface deposition conductive layer can effectively obtain electric conductivity, reduces the consumption of conductive powder body.This type of research is at present rare report also.
Summary of the invention
The object of the invention is to meet the demand of modern people to safety, a light-colored conductive attapulgite powder is provided, for preparing light-colored antistatic/conductive fiber, lay the foundation.
According to technical scheme provided by the invention, a kind of preparation method of light-colored conductive attapulgite powder, comprises the following steps:
1) take a certain amount of attapulgite, join configure there is finite concentration SnCl 4in solution;
2) ammoniacal liquor is slowly added drop-wise to the SnCl that contains attapulgite with the mol ratio of being a bit larger tham 4: 1 4in solution, be added dropwise to complete rear placement a few hours to make seed-solution, standby;
3) by SnCl 4and SbCl 3join in certain density HCl, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor, in this process, keep PH constant simultaneously;
4) filter, with deionized water, gained solid is cleaned, gained material is placed in vacuum drying chamber and is placed in Muffle furnace after dry again and calcines.
Step 1 wherein) SnCl configuring 4solution concentration is 0.01-0.1mol/L.
Step 3 wherein) concentration of hydrochloric acid using is 1-4mol/L.
Step 4 wherein) calcining heat of Muffle furnace is 500-1000 ℃, calcination time 4-10 hour.
The products characteristics of narrating in the present invention is for possessing nucleocapsid structure, and surface deposition has the light attapulgite powder of ATO conductive layer.
This technology is for the preparation with the nano-powder of conducting function, and the attapulgite powder obtaining can be applied to the preparation that light color has antistatic/conducting function fiber, meets people for the demand of safety to fabrics.
Accompanying drawing explanation
Fig. 1 is the diagram of attapulgite before processing;
Fig. 2 is the diagram after example 1 solution-treated;
Fig. 3 is the diagram after example 2 solution-treated;
Fig. 4 is the diagram after example 3 solution-treated;
Fig. 5 is the diagram after example 1 calcination processing;
Fig. 6 is the diagram after example 2 calcination processing;
Fig. 7 is the diagram after example 3 calcination processing.
Embodiment
The present invention is a kind of preparation method of light-colored conductive attapulgite, the steps include:
1) take a certain amount of attapulgite, join configure there is finite concentration SnCl 4in solution;
2) ammoniacal liquor is slowly added drop-wise to the SnCl that contains attapulgite with the mol ratio of being a bit larger tham 4: 1 4in solution, be added dropwise to complete rear placement a few hours to make seed-solution, standby;
3) by SnCl 4and SbCl 3join in certain density HCl, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor, in this process, keep PH constant simultaneously;
4) filter, with deionized water, gained solid is cleaned, gained material is placed in vacuum drying chamber and is placed in Muffle furnace after dry again and calcines.
Embodiment 1:
Take 10g attapulgite, the SnCl that to join the concentration that configures be 0.05mol/L 4in solution, ammoniacal liquor is slowly added drop-wise to the SnCl that contains attapulgite with the mol ratio of being a bit larger tham 4: 1 4in solution, be added dropwise to complete rear placement and within 4 hours, make seed-solution; By 5.80g SnCl 4with 0.85g SbCl 3join in the HCl of 2mol/L, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor simultaneously; Filter, with deionized water, gained solid is cleaned, gained material is placed in after vacuum drying chamber is dried and is placed in Muffle furnace calcining (600 ℃, 8 hours) again, and the conductivity of gained conductive powder body is 1S/cm.
Embodiment 2:
Take 15g attapulgite, in the SnCl4 solution that to join the concentration that configures be 0.1mol/L, ammoniacal liquor is slowly added drop-wise in the SnCl4 solution that contains attapulgite with the mol ratio of being a bit larger tham 4: 1, be added dropwise to complete rear placement and within 5 hours, make seed-solution; By 8.80g SnCl 4with 1.45g SbCl 3join in the HCl of 3mol/L, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor simultaneously; Filter, with deionized water, gained solid is cleaned, gained material is placed in after vacuum drying chamber is dried and is placed in Muffle furnace calcining (750 ℃, 4 hours) again, and the conductivity of gained conductive powder body is 2S/cm.
Embodiment 3:
Take 7.5g attapulgite, the SnCl that to join the concentration that configures be 0.025mol/L 4in solution, ammoniacal liquor is slowly added drop-wise to the SnCl that contains attapulgite with the mol ratio of being a bit larger tham 4: 1 4in solution, be added dropwise to complete rear placement and within 3 hours, make seed-solution; By 4.40g SnCl 4with 0.85g SbCl 3join in the HCl of 2mol/L, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor simultaneously; Filter, with deionized water, gained solid is cleaned, gained material is placed in after vacuum drying chamber is dried and is placed in Muffle furnace calcining (800 ℃, 4 hours) again, and the conductivity of gained conductive powder body is 0.5S/cm.

Claims (4)

1. a preparation method for light-colored conductive attapulgite powder, is characterized in that, at stibium doping stannic oxide (ATO) conductive layer of attapulgite's surface deposition one deck light color, the steps include:
1) take a certain amount of attapulgite, join configure there is finite concentration SnCl 4in solution;
2) ammoniacal liquor is slowly added drop-wise to the SnCl that contains attapulgite with the mol ratio of being a bit larger tham 4: 1 4in solution, be added dropwise to complete rear placement a few hours to make seed-solution, standby;
3) by SnCl 4and SbCl 3join in certain density HCl, be configured to mixed solution, be slowly added drop-wise in the seed-solution in stirring with ammoniacal liquor, in this process, keep PH constant simultaneously;
4) filter, with deionized water, gained solid is cleaned, gained material is placed in vacuum drying chamber and is placed in Muffle furnace after dry again and calcines.
2. the preparation method of light-colored conductive attapulgite powder according to claim 1, is characterized in that step 1) SnCl that configures 4solution concentration is 0.01-0.1mol/L.
3. the preparation method of light-colored conductive attapulgite powder according to claim 1, is characterized in that step 3) concentration of hydrochloric acid that uses is 1-4mol/L.
4. the preparation method of light-colored conductive attapulgite powder according to claim 1, is characterized in that step 4) calcining heat of Muffle furnace is 500-1000 ℃, calcination time 4-10 hour.
CN201410348252.3A 2014-07-18 2014-07-18 A kind of preparation method of light-colored conductive attapulgite powder Active CN104124002B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593890A (en) * 2015-02-06 2015-05-06 江苏盛虹科技股份有限公司 Attapulgite hybrid conductive fibers and preparation method thereof
CN106883704A (en) * 2017-03-09 2017-06-23 常州大学 A kind of attapulgite graphene composite conductive priming paint and preparation method thereof
CN111013559A (en) * 2019-12-25 2020-04-17 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
CN111584153A (en) * 2020-05-27 2020-08-25 江苏纳欧新材料有限公司 Method for preparing white rod-shaped conductive material by using attapulgite as template

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101000809A (en) * 2006-12-31 2007-07-18 江苏工业学院 Preparation method of nano-conducting attapulgite material
CN101423673A (en) * 2008-11-28 2009-05-06 江苏工业学院 Method for improving brightness of attapulgite
JP2011236453A (en) * 2010-05-07 2011-11-24 Toda Kogyo Corp Silver particulate and method for producing the same, conductive paste containing the silver particulates, conductive film, and electronic device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101000809A (en) * 2006-12-31 2007-07-18 江苏工业学院 Preparation method of nano-conducting attapulgite material
CN101423673A (en) * 2008-11-28 2009-05-06 江苏工业学院 Method for improving brightness of attapulgite
JP2011236453A (en) * 2010-05-07 2011-11-24 Toda Kogyo Corp Silver particulate and method for producing the same, conductive paste containing the silver particulates, conductive film, and electronic device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593890A (en) * 2015-02-06 2015-05-06 江苏盛虹科技股份有限公司 Attapulgite hybrid conductive fibers and preparation method thereof
CN104593890B (en) * 2015-02-06 2017-02-01 江苏盛虹科技股份有限公司 Attapulgite hybrid conductive fibers and preparation method thereof
CN106883704A (en) * 2017-03-09 2017-06-23 常州大学 A kind of attapulgite graphene composite conductive priming paint and preparation method thereof
CN111013559A (en) * 2019-12-25 2020-04-17 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
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
CN111584153A (en) * 2020-05-27 2020-08-25 江苏纳欧新材料有限公司 Method for preparing white rod-shaped conductive material by using attapulgite as template

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