CN1470623A - Electrorheological liquid of kaolinke/carboxymethyl starch interposed layer composite material - Google Patents

Electrorheological liquid of kaolinke/carboxymethyl starch interposed layer composite material Download PDF

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Publication number
CN1470623A
CN1470623A CNA02114690XA CN02114690A CN1470623A CN 1470623 A CN1470623 A CN 1470623A CN A02114690X A CNA02114690X A CN A02114690XA CN 02114690 A CN02114690 A CN 02114690A CN 1470623 A CN1470623 A CN 1470623A
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kaolin
carboxymethyl starch
intercalation
composite material
starch
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CN1205322C (en
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赵晓鹏
王宝祥
李佳
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The present invention relates to a new-type electro-rheologic fluid material obtained by means of interaction of kaoline and carboxymethyl starch. Its preparation method includes the following steps: selecting and using dimethyl sulfoxide as precursor, preparing kaoline/dimethyl sulfoxide intercalation composite, utilizing secondary intercalation substitution of carboxmethyl starch to make the carboxymethyl starch be inserted into interlayer of kaoline and make the flake layer of kaoline be stripped, so that the single flake layer of kaoline can be dispersed in the carboxymethyl starch so as to form the homogeneized phase material with nano size. It has higher mechanical value, wide working temperature zone and good antisettling property.

Description

Kaolin/carboxymethyl starch intercalation composite material electrorheological fluid
The present invention relates to a kind of kaolin/carboxymethyl starch intercalation composite material electrorheological fluid.
Electrorheological fluid (Electrorheological Fluid is called for short the ER fluid) is a kind of novel intelligent material, has great application prospect in fields such as vibration damping, mechanical transmission, automatic control, electromechanical integration.At present, the performance of electrorheological fluid does not also reach the practicability requirement, and wherein topmost restraining factors are: the mechanics value under the electric field excitation is not high and resistance to settling is relatively poor.Research about the electrorheological fluid discrete state material concentrates in inorganic oxide and two fields of organic high molecular polymer material mostly.Mineral-type materials once was the main research object of electrorheological fluid, and European patent EP 0396237 is utilized the dispersion particle of silico-aluminate as electrorheological fluid, and its composition is (Al 2O 3) b(SiO 2) c, b: c but exists mechanical property on the low side in 1: 1~1: 9 scope, and sedimentation resistance stability is poor, to shortcomings such as equipment attrition are big; The disperse phase that many afterwards employing organic high molecular polymer materials are electrorheological fluid is (as H.Block and J.P.Kelly, U.K.Patent, 2170510 (1985)), although its mechanics value is better than inorganic materials height and resistance to settling usually, but complicated process of preparation, the cost height, the toxicity that has is big, is difficult to realize industrialization.
The purpose of this invention is to provide the interactional novel electrorheological liquid of a kind of kaolin and carboxymethyl starch material, its disperse phase is kaolin/carboxymethyl starch intercalation composite material.Adopt the secondary intercalation method of substitution, selected for use dimethyl sulfoxide (DMSO) to make presoma, at first prepare the kaolin intercalated compound; Secondary intercalation through carboxymethyl starch replaces then, and carboxymethyl starch is inserted the kaolin interlayer, makes the kaolin limellar stripping.The single lamella of kaolin is dispersed in the carboxymethyl starch, forms the homogeneous phase material on the nanoscale.This exfoliated kaolin/carboxymethyl starch intercalation composite material had both had higher mechanics value, wide operation temperature area and good resistance to settling, and characteristics such as cheap cost, simple preparation technology are arranged again.Giving full play to the different specialities of organic materials and inorganic materials, realized mutual supplement with each other's advantages, is a kind of er material of high comprehensive performance.
The concrete enforcement of the object of the invention is as follows: get a certain amount of kaolin and be scattered in the dimethyl sulphoxide solution, stirred one day between 60-80 ℃, get kaolin/carboxymethyl starch intercalated compound.Add starch and dehydrated alcohol in three-necked bottle, add a certain amount of KOH between 30-40 ℃, add-on is about half of the total consumption of KOH, and starch is carried out activation treatment.After reacting half an hour, add KOH and chloroacetic acid mixture and also be warming up to 40-50 ℃, reacted 3 hours.The reaction finish after, suction filtration, filter cake with absolute ethanol washing repeatedly, drying and crushing get final product carboxymethyl starch.Be scattered in the distilled water kaolin mixture that makes and stirring, make it abundant swelling, pour into and form first component in the three-necked bottle, again carboxymethyl starch is fully dissolved with distilled water, move in the separating funnel, form second component.On heating jacket, the kaolin mixture is stirred, be heated to and begin to drip carboxymethyl starch soln about 60 ℃, dropwise the back homo(io)thermism between 70-80 ℃, reacted 8 hours, after having reacted, suction filtration uses absolute ethanol washing more than 3 times.60 ℃ of following vacuum-dryings of filter cake 3 hours obtain the light gray particle 80 ℃ of following half an hour, are ground into fine particle with mortar, get final product kaolin/carboxymethyl starch intercalated compound.The composite particles that makes is put into agate mortar, grind to form tiny and uniform particle.Silicone oil 100 ℃ dry one hour down, particle 31% mixes with silicone oil that can to obtain with kaolin/carboxymethyl starch mixture be the electrorheological fluid of dispersion particle by volume.
Implementation procedure of the present invention and material property are described in detail by following examples and accompanying drawing:
Embodiment one (kaolin/carboxymethyl starch composite material by electric current becomes liquid):
In the process of preparation kaolin/carboxymethyl starch intercalated compound, adopted the method that replaces intercalation, promptly insert the kaolin interlayer with the presoma dimethyl sulfoxide (DMSO) earlier, with carboxymethyl starch presoma is replaced out again, form kaolin/carboxymethyl starch intercalated compound.Get 10g kaolin in the experiment and be scattered in the 20ml dimethyl sulphoxide solution, 60-80 ℃ of following stirring reaction one day can get the kaolin intercalated compound.In three-necked flask, add 10g starch and 40ml dehydrated alcohol, fully stir.Add 1.5gKOH in the time of 30-40 ℃, add-on is half of the total consumption of KOH (3g), starch is carried out alkalinisation treatment, after half an hour, add 1.5gKOH and 5g chloroacetic acid mixture and be warming up to 40-50 ℃, the carboxymethylation processing was carried out in reaction in 3 hours under this temperature.The reaction finish after, suction filtration, filter cake with absolute ethanol washing repeatedly, drying and crushing get final product carboxymethyl starch.Be scattered in the distilled water kaolin mixture that makes and stirring, make it abundant swelling, pour into and form first component in the three-necked flask; Again carboxymethyl starch is fully dissolved with distilled water, move in the separating funnel, form second component.On heating jacket abundant swollen kaolin mixture is stirred, begin to drip carboxymethyl starch soln when being heated to 60 ℃, dropwise the back homo(io)thermism between 70-80 ℃, reaction is 8 hours under this temperature.After reaction finished, suction filtration used absolute ethanol washing more than 3 times in the process of suction filtration.After suction filtration is finished, sample is put into 60 ℃ of following vacuum-dryings of vacuum drying oven 3 hours, obtains the light gray particle 80 ℃ of down dry half an hour, be ground into fine particle with mortar, get final product kaolin/carboxymethyl starch intercalated compound.The composite particles that makes is put into agate mortar, ground 3 hours, be ground into tiny and uniform particle.Silicone oil is at 100 ℃ down after dry one hour, and particle 31% mixes with silicone oil by volume, and can obtain with kaolin/carboxymethyl starch mixture is the electrorheological fluid of dispersion particle.Fig. 1 has shown that volume ratio is that kaolin/carboxymethyl starch matrix material (ratio of components is 1: 1) electrorheological fluid of 31% is in the situation of different strength of electric field down cut stress with shear rate change.Fig. 2 is the situation of kaolin/carboxymethyl starch (ratio of components is 1: 1), carboxymethyl starch and the shear-stress of washed kaolin under different strength of electric field.Fig. 3 is under the different strength of electric field, the different proportionings of mixture and the relation between the shear-stress.
Embodiment two (washed kaolin electrorheological fluid):
With 150 ℃ down kaolin and the methyl-silicone oil behind the dry 2h be mixed with the washed kaolin electrorheological fluid by particle/silicone oil volume ratio 31%, the situation of measuring its shear-stress under different strength of electric field is as shown in Figure 1.
Embodiment three (carboxymethyl starch electrorheological fluid)
Prepare carboxymethyl starch by embodiment one, itself and methyl-silicone oil are mixed with the carboxymethyl starch electrorheological fluid by particle/silicone oil volume ratio 31%.The situation of measuring its shear-stress under different strength of electric field as shown in Figure 1.

Claims (5)

1. kaolin/carboxymethyl starch intercalation composite material electrorheological fluid.The disperse phase that it is characterized in that this material is kaolin/carboxymethyl starch intercalation composite particles, and the external phase base fluid is a methyl-silicone oil; The technology for preparing this discrete state material is selected the secondary intercalation method for use.
2. according to the described kaolin of claim 1/carboxymethyl starch intercalation composite material electrorheological fluid, it is characterized in that dispersion particle is directly to insert the kaolin interlayer by dimethyl sulfoxide (DMSO) earlier, forms organic/inorganic composite; By carboxymethyl starch this organic/inorganic composite is carried out secondary intercalation again and replace, form kaolin/carboxymethyl starch intercalation composite material.
3. according to the described kaolin of claim 1/carboxymethyl starch intercalation composite material electrorheological fluid, it is characterized in that replacing through the secondary intercalation of carboxymethyl starch, carboxymethyl starch is inserted the kaolin interlayer, makes the kaolin limellar stripping; The single lamella of kaolin is dispersed in the carboxymethyl starch, forms the homogeneous phase material on the nanoscale.
4. according to the described kaolin of claim 1/carboxymethyl starch intercalation composite material electrorheological fluid, it is characterized in that kaolin/carboxymethyl starch intercalation composite material particle 31% mixes with silicone oil that to obtain with kaolin/carboxymethyl starch mixture be the electrorheological fluid of dispersion particle by volume.
5. according to the described kaolin of claim 1/carboxymethyl starch intercalation composite material electrorheological fluid, it is characterized in that preparation technology's method may further comprise the steps:
(1) select for use kaolin, dimethyl sulfoxide (DMSO), starch, methyl-silicone oil etc. as raw material;
(2) get a certain amount of kaolin and be scattered in the dimethyl sulphoxide solution, 60-80 ℃ was stirred one day down, gets kaolin/carboxymethyl starch intercalated compound;
(3) add starch and dehydrated alcohol in three-necked bottle, add a certain amount of KOH in the time of 30-40 ℃, add-on is about half of the total consumption of KOH, and starch is carried out activation treatment; After reacting half an hour, add KOH and chloroacetic acid mixture and also be warming up to 40-50 ℃, reacted 3 hours; The reaction finish after, suction filtration, filter cake with absolute ethanol washing repeatedly, drying and crushing get final product carboxymethyl starch;
(4) the kaolin mixture that makes is scattered in the distilled water and stirring, makes it abundant swelling, pour into and form first component in the three-necked bottle, again carboxymethyl starch is fully dissolved with distilled water, move in the separating funnel, form second component; On heating jacket the kaolin mixture is stirred, begin to drip carboxymethyl starch soln when being heated to 60 ℃, dropwise the back homo(io)thermism between 70-80 ℃, reacted 8 hours, after having reacted, suction filtration uses absolute ethanol washing more than 3 times; 60 ℃ of following vacuum-dryings of filter cake 3 hours obtain the light gray particle 80 ℃ of following half an hour, are ground into fine particle with mortar, get final product kaolin/carboxymethyl starch intercalated compound;
(5) composite particles that makes is put into agate mortar, grind to form tiny and uniform particle; Silicone oil 100 ℃ dry one hour down, particle 31% mixes with silicone oil that can to obtain with kaolin/carboxymethyl starch mixture be the electrorheological fluid of dispersion particle by volume.
CN 02114690 2002-07-22 2002-07-22 Electrorheological liquid of kaolinke/carboxymethyl starch interposed layer composite material Expired - Fee Related CN1205322C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100448966C (en) * 2004-11-03 2009-01-07 西北工业大学 Titanium oxide/formamide/carboxymethyl starch/core-shell type nanometer electrorheological material
CN101323808B (en) * 2007-06-15 2010-12-08 西北工业大学 Potato expansion starch carbonizing porous carbon ER fluid material
CN103926119A (en) * 2014-02-19 2014-07-16 中国矿业大学(北京) Method for preparing kaolinite with high radius-thickness ratio, and measuring and calculating radius-thickness ratio of kaolinite
CN112500148A (en) * 2020-11-27 2021-03-16 天长市中德电子有限公司 Preparation method of high-coercivity strontium ferrite magnetic material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100448966C (en) * 2004-11-03 2009-01-07 西北工业大学 Titanium oxide/formamide/carboxymethyl starch/core-shell type nanometer electrorheological material
CN101323808B (en) * 2007-06-15 2010-12-08 西北工业大学 Potato expansion starch carbonizing porous carbon ER fluid material
CN103926119A (en) * 2014-02-19 2014-07-16 中国矿业大学(北京) Method for preparing kaolinite with high radius-thickness ratio, and measuring and calculating radius-thickness ratio of kaolinite
CN112500148A (en) * 2020-11-27 2021-03-16 天长市中德电子有限公司 Preparation method of high-coercivity strontium ferrite magnetic material

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