CN105949506B - An a kind of one step preparation method of hydrophobic Yi Meng clays - Google Patents
An a kind of one step preparation method of hydrophobic Yi Meng clays Download PDFInfo
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- CN105949506B CN105949506B CN201610299050.3A CN201610299050A CN105949506B CN 105949506 B CN105949506 B CN 105949506B CN 201610299050 A CN201610299050 A CN 201610299050A CN 105949506 B CN105949506 B CN 105949506B
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- Prior art keywords
- hydrophobic
- meng
- modifying agent
- step preparation
- meng clays
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000004927 clay Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000012065 filter cake Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 241000446313 Lamella Species 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000004075 alteration Effects 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical class [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000005341 cation exchange Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000000524 functional group Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052900 illite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/42—Clays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Abstract
An a kind of one step preparation method of hydrophobic Yi Meng clays, belongs to Yi Meng clay production technical fields.Comprise the following steps：Modifying agent is added in alcohol solution first, stirring adds Yi Meng clay powders after being completely dispersed uniformly, and slurries are obtained in 60~80 DEG C of reactions；Then the above-mentioned slurries by step are filtered, the drying grinding of obtained filter cake is can obtain into hydrophobic Yi Meng clays powder.The powder obtained by the present invention has more preferable hydrophobic performance and hydrophobic performance is stable, has good compatibility with organic matter, can be dispersed in the polymer.Preparation method technique provided by the invention is simple, and cost is cheap, and preparation efficiency is high.
Description
Technical field：
The present invention relates to Yi Meng clay production technical fields, and in particular to a kind of preparation method of hydrophobic Yi Meng clays
Background technology：
Natural Iraq/Mongolia mixed layer clay mineral be aqueous phyllosilicate, is a kind of by montmorillonite lamella and illite lamella
The transiens mineral formed by different proportion along C axles, its basic structural feature are silicon-oxy tetrahedron lamella and aluminum oxide octahedral sheet
Layer infinitely extends on a, b direction of structure cell, and rule repeats, piece and piece composition structural unit layer, in the c-direction without translation week
Phase.Because the lattice position of some silicon atoms is occupied by the iron and aluminium of some low price, thus cause lamella negatively charged, interlayer by
The metal cations such as calcium ion, sodium ion balance the uncharged group such as negative electricity, also a number of hydroxyl.Wherein interlayer sun
Ion can swap with some other groups, and with organic matters such as coupling agents dehydrating condensation can occur for hydroxyl.
Due to the lamellar structure and fire resistance of clay, the barrier property of polymer can be improved by being applied in polymer
And fire resistance.But natural Iraq/Mongolia mixed layer clay mineral good hydrophilic property, water-swellable, it is difficult in organic system compatible.Cause
This in use, must be modified to natural Yi Meng clays, makes its surface switch to hydrophobic, Neng Gouyu by hydrophilic in organic system
Polymer-compatible.
Existing organoclay method is usually to carry out cation exchange, cation exchange using cationic surfactant
Method be generally modified in pure water, can produce a large amount of bubbles, reduce products collection efficiency and simultaneously made troubles to production, and this
Method only slightly reduces the hydrophily of clay minerals, not only not up to hydrophobicity (water contact angle be more than 90 °), and with
Time elapses, and contact angle also occurs that further decline.Therefore the organic clay obtained in general using this method can not be with
Polymer combines well, and its organic compatibility needs further to be improved.
The content of the invention：
It is an object of the invention to solve problems of the prior art, there is provided a kind of Yi Meng with hydrophobic effect glues
One one step preparation method of soil, its step are as follows：
Modifying agent is added in alcohol solution, stirring adds Yi Meng clay powders after being completely dispersed uniformly, at 60~80 DEG C
Reaction obtains slurries；Slurries are filtered, the drying grinding of obtained filter cake is obtained into hydrophobic Yi Meng clays powder.
In such scheme, modifying agent used is oxyalkylsiloxane, preferably is selected from DOW CORNING Z6173 or DOW CORNING 11-100
Any one.
Preferably, the volume ratio of ethanol and water used in the alcohol solution of preparation is (1~3)：1.
In any of the above-described scheme preferably, the time of reaction is 1~4 hour.
In any of the above-described scheme, modifier concentration is to correspond to 0.05-0.3g modifying agent, preferred pair per 10ml alcohol solutions
Answer 0.1~0.2g modifying agent.
In any of the above-described scheme preferably, modifying agent add quality for Yi Meng clay powder qualities 16%~
50%.
In any of the above-described scheme preferably, modifying agent add quality for Yi Meng clay powder qualities 17%~
30%.
In any of the above-described scheme preferably, modifying agent add quality for Yi Meng clay powder qualities 17%~
25%.
In any of the above-described scheme preferably, modifying agent add quality for Yi Meng clay powder qualities 17%~
20%.
In any of the above-described scheme preferably, modifying agent add quality for Yi Meng clay powder qualities 18%~
19%.
In any of the above-described scheme preferably, ultrasonic vibration can also be carried out after clay stirring is added.
In any of the above-described scheme preferably, the time for ultrasonic vibration being carried out after clay stirring is added is 5~20 points
Clock.
In any of the above-described scheme preferably, can be washed with deionized during filtering.
In any of the above-described scheme preferably, drying temperature is 70~120 DEG C.
In any of the above-described scheme preferably, drying temperature is 80~110 DEG C.
Beneficial effect：
1 can fully confirm that obtained hydrophobic Yi Meng clays have moderately good hydrophobic effect by Fig. 1 Fig. 2.
The 2 hydrophobic Yi Meng clays being prepared by the method for the present invention have excellent organic compatibility, can be dispersed in poly-
Composite is formed in compound, strengthens the barrier property and fire resistance of composite.
3 preparation methods are simple, avoid caused a large amount of foams, low for equipment requirements and yield in preparation process high.
Brief description of the drawings
Contact angle photo before Yi Meng clay alterations in Fig. 1 present invention；Powder water-swellable in Fig. 1, contact angle are 0 °
Fig. 2 is that contact angle photo, middle water droplet keep the form in photo after Yi Meng clay alterations in the present invention, and contact angle is
108°。
Fig. 3 is infrared spectrogram, wherein 2962cm before and after Yi Meng clay alterations in the present invention-1The absworption peak at place is that-CH is anti-
Symmetrical stretching vibration absworption peak.And-CH is organo-functional group, therefore this functional group is not present on unmodified Yi Meng clays.In addition
3400cm-1Neighbouring peak is the-OH stretching vibration peaks of physical absorption water, and the peak is decreased obviously in modified infrared spectrogram.
Embodiment：
Further specific descriptions are done to the present invention with reference to embodiments, but are not limited to these embodiments.
Modifying agent used in embodiment use is bought from Daukangnin GmbH.
Embodiment 1
It is 1 that 1g DOW CORNINGs Z6173 is added into 90ml alcohol water ratio at room temperature：In 1 solution, stir to DOW CORNING Z6173
It is dispersed in solution.Then 5g Yi Meng clays are added in above-mentioned solution, be uniformly mixed.Slurries will be obtained to be transferred to
Three-necked flask, 70 DEG C of water-baths 2 hours, filtration washing, 80 DEG C of drying and grindings obtain hydrophobic Yi Meng clays powder, measure it and connect
Feeler is 93 °, and measures in 1 hour and do not decline.
Embodiment 2
It is 2 that 0.9g DOW CORNINGs Z6173 is added into 90ml alcohol water ratio at room temperature：In 1 solution, stir to DOW CORNING
Z6173 is dispersed in solution.Then 5g Yi Meng clays are added in above-mentioned solution, be uniformly mixed.Slurries will be obtained
It is transferred to three-necked flask, 70 DEG C of water-baths 2 hours, filtration washing, 110 DEG C of drying and grindings obtain hydrophobic Yi Meng clays powder,
Its contact angle is measured as 106 °, and measures in 1 hour and does not decline.
Embodiment 3
It is 1 that 1g DOW CORNINGs Z6173 is added into 90ml alcohol water ratio at room temperature：In 1 solution, stir to DOW CORNING Z6173
It is dispersed in solution.Then 5g Yi Meng clays are added in above-mentioned solution, be uniformly mixed, and ultrasonic disperse 10 divides
Clock.Slurries will be obtained and be transferred to three-necked flask, 70 DEG C of water-baths 2 hours, filtration washing, 80 DEG C of drying and grindings obtain it is hydrophobic she
Clay powder is covered, measures its contact angle as 95 °, and measure in 1 hour and do not decline.
Comparative example 1
It is 2 that 0.5g cetyl trimethylammonium bromides are added into 90ml alcohol water ratio at room temperature：In 1 solution, stirring is extremely
Cetyl trimethylammonium bromide is completely dissolved.5g Yi Meng clays are added in above-mentioned solution, are uniformly mixed.It will be starched
Liquid is transferred to three-necked flask, and 60 DEG C of water-baths 2 hours, filtration washing drying and grinding obtains final powder.Measure its contact angle
For 51.2 °, 0 ° was dropped in 10 minutes.
Comparative example 2
It is 1 that 0.2g DOW CORNINGs Z6173, which adds 90ml alcohol water ratio,：In 2 solution, stir to Z6173 and mix in the solution point
Dissipate uniformly, 5g Yi Meng clays are added in solution, is uniformly mixed, is obtained slurries and be transferred to three-necked flask, 60 DEG C of water-baths are anti-
Answer 2 hours, filtration drying grinds to obtain final powder, measures its contact angle as 23 °, and contact angle continuous decrease is extremely in 1 minute
0°。
Comparative example 3
It is 4 that 1g DOW CORNINGs Z6173 is added into 90ml alcohol water ratio at room temperature：In 1 solution, stir to DOW CORNING Z6173
It is dispersed in solution.Then 5g Yi Meng clays are added in above-mentioned solution, be uniformly mixed.Slurries will be obtained to be transferred to
Three-necked flask, 50 DEG C of water-baths 2 hours, filtration washing, 110 DEG C of drying and grindings obtain hydrophobic Yi Meng clays powder, measure it
Contact angle is 59 °, and contact angle continuous decrease is 0 ° in 5 minutes.
Heretofore described specific implementation case is only the preferable case study on implementation of the present invention, is not used for limiting this hair
Bright practical range.The equivalent changes and modifications made according to the content of scope of the present invention patent, all should be used as the present invention
Technology category.
Claims (9)
- A 1. a kind of one step preparation method of hydrophobic Yi Meng clays, it is characterised in that step is as follows：Modifying agent is added in alcohol solution, the volume ratio of ethanol and water used in the alcohol solution of preparation is (1~3)：L, stir Mix and add Yi Meng clay powders after being completely dispersed uniformly, slurries are obtained in 60~80 DEG C of reactions；Slurries are filtered, will be obtained Filter cake drying grinding obtain hydrophobic Yi Meng clays powder；Modifying agent used is oxyalkylsiloxane.
- An a kind of 2. one step preparation method of hydrophobic Yi Meng clays according to claim 1, it is characterised in that modifying agent used For any one in DOW CORNING Z6173 or DOW CORNING 11-100.
- An a kind of 3. one step preparation method of hydrophobic Yi Meng clays according to claim 1, it is characterised in that the time of reaction For 1~4 hour.
- An a kind of 4. one step preparation method of hydrophobic Yi Meng clays according to claim 1, it is characterised in that modifier concentration 0.05-0.3g modifying agent is corresponded to for every 10ml alcohol solutions.
- An a kind of 5. one step preparation method of hydrophobic Yi Meng clays according to claim l, it is characterised in that modifier concentration For the corresponding 0.1~0.2g modifying agent of every 10ml alcohol solutions.
- A 6. one step preparation method of a kind of hydrophobic Yi Meng clays according to claim 1, it is characterised in that modifying agent adds Quality is the 16%~50% of Yi Meng clay powder qualities.
- A 7. one step preparation method of a kind of hydrophobic Yi Meng clays according to claim 1, it is characterised in that modifying agent adds Quality is the 17%~30% of Yi Meng clay powder qualities.
- A 8. one step preparation method of a kind of hydrophobic Yi Meng clays according to claim 1, it is characterised in that adding clay The time that ultrasonic vibration is carried out after stirring is 5~20 minutes.
- A 9. one step preparation method of a kind of hydrophobic Yi Meng clays according to claim 1, it is characterised in that drying temperature is 70~120 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610299050.3A CN105949506B (en) | 2016-05-06 | 2016-05-06 | An a kind of one step preparation method of hydrophobic Yi Meng clays |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610299050.3A CN105949506B (en) | 2016-05-06 | 2016-05-06 | An a kind of one step preparation method of hydrophobic Yi Meng clays |
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| CN105949506A CN105949506A (en) | 2016-09-21 |
| CN105949506B true CN105949506B (en) | 2017-12-12 |
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| CN201610299050.3A Expired - Fee Related CN105949506B (en) | 2016-05-06 | 2016-05-06 | An a kind of one step preparation method of hydrophobic Yi Meng clays |
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| CN107227053A (en) * | 2017-06-12 | 2017-10-03 | 广西大学 | A kind of modified Yi Meng clays hydrophobic coating easy to clean and preparation method thereof |
| CN108611022B (en) * | 2018-03-22 | 2021-02-02 | 杭州方周科技有限公司 | Tire repair liquid containing illite smectite clay and preparation method thereof |
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| CN101254924A (en) * | 2008-04-09 | 2008-09-03 | 中国科学院化学研究所 | Silicane coupling agent surface grafted modified clay as well as preparation method and use thereof |
| CN101342482B (en) * | 2008-08-15 | 2011-11-16 | 淮阴师范学院 | Preparation method for concave-convex stick clay soil/polyacrylamide composite adsorption agent |
| CN101658782A (en) * | 2009-08-24 | 2010-03-03 | 淮阴师范学院 | Method for preparing adsorbent by modifying attapulgite clay |
| US20120082791A1 (en) * | 2010-10-04 | 2012-04-05 | Robert Richard Liversage | Coating Composition Amenable to Elastomeric Substrates |
| CN105381791A (en) * | 2015-11-20 | 2016-03-09 | 淮阴师范学院 | Preparation method of attapulgite-based molecular imprinting type CO2 adsorbing material |
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