CN107216492A - A kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing - Google Patents
A kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing Download PDFInfo
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- CN107216492A CN107216492A CN201710563802.7A CN201710563802A CN107216492A CN 107216492 A CN107216492 A CN 107216492A CN 201710563802 A CN201710563802 A CN 201710563802A CN 107216492 A CN107216492 A CN 107216492A
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- montmorillonite
- ethanedioic acid
- dinethylformamide
- nano composite
- magnetic agitation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/04—Starch derivatives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of nano composite water absorbing material containing montmorillonite, with N dimethylformamides, ethanedioic acid, the raw material such as montmorillonite is by gelation, paste China, the synthesis nano composite water absorbing material such as magnetic agitation.Absorbent material water absorbing properties prepared by the present invention are good.
Description
Technical field
The present invention relates to a kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing, belong to Material Field.
Background technology
Polymer based clay nanocomposites are compared with the conventional composites materials with composition, due to receiving for inorganic dispersed phase
Rice dimensional effect and good interface cohesion between matrix, so that more excellent combination property is shown, in terms of water imbibition
Performance is extremely excellent.Report that more clay nanocomposites have nylon/montmorillonoid, PS/Montmorillonite, epoxy at present
Resin/montmorillonite, polyacrylamide/montmorillonite.It is seldom about the Nano composite material of montmorillonite research report of starch grafting type.I
A kind of preparation side using starch-grafted dinethylformamide and ethanedioic acid/montmorillonite-based nano composite absorbent material is invented
Method, this method is simple, and the dinethylformamide and ethanedioic acid of synthesis/montmorillonite-based nano composite absorbent material, soaking effect are good.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of nano composite water absorbing material of montmorillonoid-containing
Preparation method, the material water absorbing properties of preparation are good.
To achieve these goals, the technical solution adopted by the present invention is：A kind of nano composite water absorbing material of montmorillonoid-containing
The preparation method of material, comprises the following steps：
Step 1, weigh montmorillonite and be added in beaker, then ultrasonic wave decentralized processing 2h, then by cetyl trimethyl bromine
Change ammonium to be added dropwise to wherein；
Step 2 and then the montmorillonite that cetyl trimethylammonium bromide is added dropwise is transferred in vacuum glove box, ultraviolet processing is anti-
2h is answered, the montmorillonite being modified with cetyl trimethylammonium bromide is obtained;
Step 3, dinethylformamide and ethanedioic acid are added to filled in deionized water beaker, ultrasonication 3h, simultaneously
Magnetic agitation;
Step 4, after dinethylformamide has dissolved add sodium carbonate in the ethanedioic acid in solution into neutrality, add shallow lake
Powder；
Step 5 and then it is warming up to 60 DEG C, magnetic agitation makes starch be gelatinized in monomer solution, while opening ultrasonication
2h;
Step 6, when solution becomes colourless from muddy milky, the montmorillonite that will be modified with cetyl trimethylammonium bromide
It is added thereto, continues magnetic agitation 2h;
Step 7, magnetic agitation are taken out after terminating from three-necked flask, are put into beaker, cool to 50 DEG C, add pentavalent vanadic salts and draw
Send out agent, gelation 3h;
Step 8,2h is stored at room temperature, produces gel bulk product, be then transferred into Muffle furnace：First 200 DEG C under nitrogen atmosphere,
2h is calcined under 0.2kpa, then in CO2Under atmosphere, 3h is calcined under 0.5kpa, starch-grafted dinethylformamide is finally given
With ethanedioic acid/montmorillonite-based nano composite absorbent material；
Step 9 and then grinding, sample preparation obtain the graininess N- dimethyl formyls of 30-50 mesh sizes with 30-50 sieve screening
Amine and ethanedioic acid/montmorillonite-based nano composite absorbent material.
Beneficial effect:A kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing of the present invention, raw material is relative to be held
Easily obtain, ethanedioic acid neutralized using dinethylformamide with part etc. is as object, and heat up gelatinization in monomer solution
Starch, object and slotting main MMT intercalations, then while be crosslinked, the water suction group that in-situ grafting polymerization is can be closed further
Connection enhancing water sorption, makes it absorb water into one its further modification in building-up process by magnetic agitation ultrasonication etc.
Step enhancing.Wherein implement 1 and produce dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 8g, cetyl trimethylammonium bromide 2ml, starch 5g, pentavalent vanadium salt initiators 1g.
Embodiment 2 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 40:16:5 sample.Dinethylformamide 40g, second
Diacid 16g, montmorillonite 5g, other raw material dosages, operating procedure is with embodiment 1.Obtained-dimethylformamide and second
Diacid/montmorillonite-based nano composite absorbent material soaking effect is best.
Embodiment
Embodiment 1 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 8g, cetyl trimethylammonium bromide 2ml, starch 5g, pentavalent vanadium salt initiators 1g.
Step 1, weigh 8g montmorillonites and be added in beaker, then ultrasonic wave decentralized processing 2h, then by 2ml cetyls
Trimethylammonium bromide is added dropwise to wherein；
Step 2 and then the montmorillonite that cetyl trimethylammonium bromide is added dropwise is transferred in vacuum glove box, ultraviolet processing is anti-
2h is answered, the montmorillonite being modified with cetyl trimethylammonium bromide is obtained;
Step 3,45g dinethylformamides and 18g ethanedioic acids are added to filled in deionized water beaker, ultrasonication
3h, while magnetic agitation;
Step 4, after dinethylformamide has dissolved add sodium carbonate in the ethanedioic acid in solution into neutrality, then add
5g starch
Step 5 and then it is warming up to 60 DEG C, magnetic agitation makes starch be gelatinized in monomer solution, while opening at ultrasonic wave
Manage 2h;
Step 6, when solution becomes colourless from muddy milky, the montmorillonite that will be modified with cetyl trimethylammonium bromide
It is added thereto, continues magnetic agitation 2h;
Step 7, magnetic agitation are taken out after terminating from three-necked flask, are put into beaker, cool to 50 DEG C, add 1g pentavalent vanadiums
Salt initiators, gelation 3h;
Step 8,2h is stored at room temperature, produces gel bulk product, be then transferred into Muffle furnace：First 200 DEG C under nitrogen atmosphere,
2h is calcined under 0.2kpa, then in CO2Under atmosphere, 3h is calcined under 0.5kpa, starch-grafted dinethylformamide is finally given
With ethanedioic acid/montmorillonite-based nano composite absorbent material；
Step 9 and then grinding, sample preparation obtain the graininess N- dimethyl formyls of 30-50 mesh sizes with 30-50 sieve screening
Amine and ethanedioic acid/montmorillonite-based nano composite absorbent material.
Embodiment 2 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 40:16:5 sample.N- dimethyl formyls
Amine 40g, ethanedioic acid 16g, montmorillonite 5g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 3 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:20:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 20g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 4 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:22:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 22g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 5 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:24:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 24g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 6 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:26:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 26g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 7, produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:10 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 10g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 8 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:12 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 12g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 9 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:14 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 14g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 10 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:16 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 16g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 11 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:18 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 18g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 12 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:20 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 20g, other raw material dosages, operating procedure is with embodiment 1.
Embodiment 13 produces dinethylformamide, ethanedioic acid, montmorillonite mass ratio 40:18:8 sample.N- dimethyl methyls
Acid amides 40g, ethanedioic acid 18g, montmorillonite 8g, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 1 produce dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 18g, montmorillonite 8g, wherein without magnetic agitation but mechanical agitation, other raw material dosages, operation step
Suddenly with embodiment 1.
Reference examples 2, produce dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl methyls
Acid amides 45g, ethanedioic acid 18g, montmorillonite 8g, wherein without ultrasonication, other raw material dosages, operating procedure is with implementing
As example 1.
Reference examples 3 produce dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 18g, montmorillonite 8g, wherein without cetyl trimethylammonium bromide modification montmorillonite, other raw materials
Consumption, operating procedure is with embodiment 1.
Reference examples 4 produce dinethylformamide, ethanedioic acid, montmorillonite mass ratio 45:18:8 sample.N- dimethyl formyls
Amine 45g, ethanedioic acid 18g, montmorillonite 8g, wherein no longer N2Calcination processing under atmosphere but under air, other raw material dosages, behaviour
Make step with embodiment 1.
Reference examples 5 produce ethanedioic acid, montmorillonite mass ratio 18:8 sample.Ethanedioic acid 18g, montmorillonite 8g,.It is added without N-
Dimethylformamide, other raw material dosages, operating procedure is with embodiment 1.
Reference examples 6 produce dinethylformamide, ethanedioic acid mass ratio 45:18 sample.Dinethylformamide 45g, second
Diacid 18g, is added without montmorillonite, other raw material dosages, and operating procedure is with embodiment 1.
Experiment test：Liquid absorbency rate is determined using natural filtration method.Accurately weigh a certain amount of starch-grafted N- diformazans
Base formamide and ethanedioic acid/montmorillonite-based nano composite absorbent material are placed in beaker, add distilled water, are stood at room temperature after 48h,
Remaining liquid is filtered with screen cloth, starch-grafted dinethylformamide and ethanedioic acid/montmorillonite after imbibition is accurately weighed
The quality of nano composite water absorbing material, liquid absorbency rate is calculated by formula (1):Q =( m2 -m 1 )/m 1(1) wherein Q
For liquid absorbency rate, g/g; m1It is that starch-grafted dinethylformamide before imbibition and ethanedioic acid/montmorillonite-based nano are compound
The quality of absorbent material, g; m2To absorb starch-grafted dinethylformamide and ethanedioic acid/montmorillonite-based nano after liquid
Composite absorbent material（g）
The natural filtration method of table one determines liquid absorbency rate result
Test result indicates that：It can be found that comparative example, embodiment 1, starch-grafted dinethylformamide and second made from 2
Diacid/montmorillonite-based nano composite absorbent material soaking effect is best.Illustrate the raw material proportioning, operating procedure is high most beneficial for synthesis
The starch-grafted dinethylformamide and ethanedioic acid of performance/montmorillonite-based nano composite absorbent material.It is obtained under other techniques
Starch-grafted dinethylformamide and ethanedioic acid/montmorillonite-based nano composite absorbent material soaking effect are general.Comparative example
1, comparative example 1,2,3,4,5,6 is can be found that.Without magnetic agitation, ultrasonic wave, at cetyl trimethylammonium bromide modification
Manage montmorillonite, N2Calcination processing under atmosphere but under air, be added without dinethylformamide, the obtained carboxylic second of montmorillonite processing
Base cellulose-benzyl acid amides/Si composite high-water-absorptivresin material soaking effects are all bad.
Claims (2)
1. a kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing, it is characterised in that with dinethylformamide, second
Diacid, the raw material such as montmorillonite is by gelation, paste China, synthesis dinethylformamide and the ethanedioic acid/montmorillonite such as magnetic agitation
Nano composite water absorbing material.
2. a kind of preparation method of the nano composite water absorbing material of montmorillonoid-containing, it is characterised in that comprise the following steps：
Step 1, weigh montmorillonite and be added in beaker, then ultrasonic wave decentralized processing 2h, then by cetyl trimethyl bromine
Change ammonium to be added dropwise to wherein；
Step 2 and then the montmorillonite that cetyl trimethylammonium bromide is added dropwise is transferred in vacuum glove box, ultraviolet processing is anti-
2h is answered, the montmorillonite being modified with cetyl trimethylammonium bromide is obtained;
Step 3, dinethylformamide and ethanedioic acid are added to filled in deionized water beaker, ultrasonication 3h, simultaneously
Magnetic agitation;
Step 4, after dinethylformamide has dissolved add sodium carbonate in the ethanedioic acid in solution into neutrality, then add
Starch；
Step 5 and then it is warming up to 60 DEG C, magnetic agitation makes starch be gelatinized in monomer solution, while opening ultrasonication
2h;
Step 6, when solution becomes colourless from muddy milky, the montmorillonite that will be modified with cetyl trimethylammonium bromide
It is added thereto, continues magnetic agitation 2h;
Step 7, magnetic agitation are taken out after terminating from three-necked flask, are put into beaker, cool to 50 DEG C, add pentavalent vanadic salts and draw
Send out agent, gelation 3h;
Step 8,2h is stored at room temperature, produces gel bulk product, be then transferred into Muffle furnace：First 200 DEG C under nitrogen atmosphere,
2h is calcined under 0.2kpa, then in CO2Under atmosphere, 3h is calcined under 0.5kpa, starch-grafted dinethylformamide is finally given
With ethanedioic acid/montmorillonite-based nano composite absorbent material；
Step 9 and then grinding, sample preparation obtain the graininess N- dimethyl formyls of 30-50 mesh sizes with 30-50 sieve screening
Amine and ethanedioic acid/montmorillonite-based nano composite absorbent material.
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Cited By (1)
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| CN107602932A (en) * | 2017-10-19 | 2018-01-19 | 宁波智果科技咨询服务有限公司 | A kind of preparation method of carboxyethyl cellulose benzyl acid amides/Si composite high-water-absorptivresin materials |
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| CN107602932A (en) * | 2017-10-19 | 2018-01-19 | 宁波智果科技咨询服务有限公司 | A kind of preparation method of carboxyethyl cellulose benzyl acid amides/Si composite high-water-absorptivresin materials |
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