CN104124002B - A kind of preparation method of light-colored conductive attapulgite powder - Google Patents

A kind of preparation method of light-colored conductive attapulgite powder Download PDF

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CN104124002B
CN104124002B CN201410348252.3A CN201410348252A CN104124002B CN 104124002 B CN104124002 B CN 104124002B CN 201410348252 A CN201410348252 A CN 201410348252A CN 104124002 B CN104124002 B CN 104124002B
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solution
attapulgite
sncl
added
light
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CN104124002A (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 kind of preparation method of light-colored conductive attapulgite powder, by a certain amount of attapulgite, the SnCl configured is added to4In solution;Ammoniacal liquor is slowly dropped to the SnCl containing attapulgite4A few hours obtained surface deposition is placed in solution, after being added dropwise to complete Sn (OH)4The attapulgite solution of crystal seed, by SnCl4And SbCl3It is added in certain density hydrochloric acid, is configured to mixed solution, is slowly dropped to simultaneously in the above-mentioned seed-solution in stirring with ammoniacal liquor;Filtering, is cleaned gained solid with deionized water, and gained material is placed in be placed in Muffle furnace again after drying in vacuum drying chamber and calcined, you can obtains corresponding light-colored conductive attapulgite powder.

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
Raising with living standards of the people and the requirement to quality of the life improve, for the need of antistatic/conductive fabric Continuous expansion is asked, traditional dark carbon system antistatic/conductive fiber has been unable to meet demand, needs exploitation light-colored antistatic/lead badly Electric fiber.A kind of preparation of this technology invention for light-colored antistatic/conductive fiber, it is proposed that new light-colored conductive attapulgite The preparation method of powder, laid the foundation for the preparation of light-colored antistatic/conductive fiber.
The shape of conductive filler has larger shadow for the performance of conductive polymeric composite and the materials of filler Ring.To reduce the dosage of conductive filler, selection rod conductive filler is typically chosen.Attapulgite is that one kind has one-dimensional rod-like knot The natural clay of structure, while depositing conductive layer on its surface as core using attapulgite effectively can obtain electric conductivity, Reduce the dosage of conductive powder body.Such also rare report of research at present.
The content of the invention
The purpose of the present invention is that meet the needs of modern people are to safety, there is provided a light-colored conductive attapulgite powder, is Light-colored antistatic/conductive fiber is prepared to lay the foundation.
According to technical scheme provided by the invention, a kind of preparation method of light-colored conductive attapulgite powder, including it is following Step:
1) weigh a certain amount of attapulgite, be added to configured there is finite concentration SnCl4In solution;
2) ammoniacal liquor is slowly dropped to the SnCl containing attapulgite with the mol ratio slightly larger than 4: 14In solution, drip Seed-solution is made into rear placement a few hours, it is standby;
3) by SnCl4And SbCl3It is added in certain density HCl, is configured to mixed solution, is slowly dripped simultaneously with ammoniacal liquor It is added in the seed-solution in stirring, keeps PH constant in the process;
4) filter, cleaned gained solid with deionized water, gained material is placed in vacuum drying chamber and is placed in again after drying Calcined in Muffle furnace.
The SnCl that wherein step 1) is configured4Solution concentration is 0.01-0.1mol/L.
Wherein concentration of hydrochloric acid used in step 3) is 1-4mol/L.
Wherein the calcining heat of step 4) Muffle furnace is 500-1000 DEG C, calcination time 4-10 hours.
In the products characteristics that the present invention is described to possess core shell structure, surface deposition has the light color of ATO conductive layers concavo-convex Rod soil powder.
This technology is directed to the preparation of the nano-powder with conducting function, and the attapulgite powder obtained can apply to Light color has the preparation of antistatic/conducting function fiber, meets the needs of people are for safety to fabrics.
Brief description of the drawings
Fig. 1 is the diagram of before processing attapulgite;
Fig. 2 is the diagram after the processing of the solution of example 1;
Fig. 3 is the diagram after the processing of the solution of example 2;
Fig. 4 is the diagram after the processing of the solution of example 3;
Fig. 5 is the diagram after the calcination processing of example 1;
Fig. 6 is the diagram after the calcination processing of example 2;
Fig. 7 is the diagram after the calcination processing of example 3.
Embodiment
The present invention is a kind of preparation method of light-colored conductive attapulgite, and its step is:
1) weigh a certain amount of attapulgite, be added to configured there is finite concentration SnCl4In solution;
2) ammoniacal liquor is slowly dropped to the SnCl containing attapulgite with the mol ratio slightly larger than 4: 14In solution, drip Seed-solution is made into rear placement a few hours, it is standby;
3) by SnCl4And SbCl3It is added in certain density HCl, is configured to mixed solution, is slowly dripped simultaneously with ammoniacal liquor It is added in the seed-solution in stirring, keeps PH constant in the process;
4) filter, cleaned gained solid with deionized water, gained material is placed in vacuum drying chamber and is placed in again after drying Calcined in Muffle furnace.
Embodiment 1:
10g attapulgites are weighed, are added to the SnCl that the concentration configured is 0.05mol/L4In solution, by ammoniacal liquor with slightly Mol ratio more than 4: 1 is slowly dropped to the SnCl containing attapulgite4Placed in solution, after being added dropwise to complete 4 hours and crystalline substance is made Kind solution;By 5.80g SnCl4With 0.85g SbCl3It is added in 2mol/L HCl, is configured to mixed solution, with ammoniacal liquor simultaneously It is slowly dropped in the seed-solution in stirring;Filtering, is cleaned gained solid with deionized water, gained material is placed in vacuum and done Calcining (600 DEG C, 8 hours) in Muffle furnace is placed in after being dried in dry case again, the electrical conductivity of gained conductive powder body is 1S/cm.
Embodiment 2:
15g attapulgites are weighed, it is in 0.1mol/L SnCl4 solution, by ammoniacal liquor with slightly to be added to the concentration configured Mol ratio more than 4: 1 is slowly dropped in the SnCl4 solution containing attapulgite, is placed after being added dropwise to complete 5 hours and crystalline substance is made Kind solution;By 8.80g SnCl4With 1.45g SbCl3It is added in 3mol/L HCl, is configured to mixed solution, with ammoniacal liquor simultaneously It is slowly dropped in the seed-solution in stirring;Filtering, is cleaned gained solid with deionized water, gained material is placed in vacuum and done Calcining (750 DEG C, 4 hours) in Muffle furnace is placed in after being dried in dry case again, the electrical conductivity of gained conductive powder body is 2S/cm.
Embodiment 3:
7.5g attapulgites are weighed, are added to the SnCl that the concentration configured is 0.025mol/L4In solution, by ammoniacal liquor with Mol ratio slightly larger than 4: 1 is slowly dropped to the SnCl containing attapulgite4Place 3 hours and be made in solution, after being added dropwise to complete Seed-solution;By 4.40g SnCl4With 0.85g SbCl3It is added in 2mol/L HCl, is configured to mixed solution, it is same with ammoniacal liquor When be slowly dropped to stirring in seed-solution in;Filtering, is cleaned gained solid with deionized water, gained material is placed in vacuum Calcining (800 DEG C, 4 hours) in Muffle furnace is placed in after being dried in drying box again, the electrical conductivity of gained conductive powder body is 0.5S/cm.

Claims (1)

1. a kind of preparation method of light-colored conductive attapulgite powder, it is characterized in that attapulgite's surface deposit one layer it is light Stibium doping stannic oxide (ATO) conductive layer, its step are:
1) weigh a certain amount of attapulgite, be added to configured there is finite concentration SnCl4In solution;
2) ammoniacal liquor is slowly dropped to the SnCl containing attapulgite with the mol ratio slightly larger than 4: 14In solution, after being added dropwise to complete A few hours obtained seed-solution is placed, it is standby;
3) by SnCl4And SbCl3It is added in certain density HCl, is configured to mixed solution, is slowly dropped to simultaneously with ammoniacal liquor In seed-solution in stirring, keep PH constant in the process;
4) filter, cleaned gained solid with deionized water, gained material is placed in vacuum drying chamber and is placed in Muffle again after drying Calcined in stove;
The SnCl that step 1) is configured4Solution concentration is 0.01-0.1mol/L;
Concentration of hydrochloric acid used in step 3) is 1-4mol/L;
The calcining heat of step 4) Muffle furnace is 500-1000 DEG C, calcination time 4-10 hours.
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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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
CN106883704B (en) * 2017-03-09 2019-10-01 常州大学 A kind of attapulgite-graphene composite conductive priming paint and preparation method thereof
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
CN111584153B (en) * 2020-05-27 2021-06-18 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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CN100550213C (en) * 2006-12-31 2009-10-14 江苏工业学院 A kind of preparation method of nano-conducting attapulgite material
CN101423673B (en) * 2008-11-28 2011-12-28 江苏工业学院 Method for improving brightness of attapulgite
JP5761483B2 (en) * 2010-05-07 2015-08-12 戸田工業株式会社 Silver fine particles and production method thereof, and conductive paste, conductive film and electronic device containing the silver fine particles

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