CN106365171B - A kind of quick Ludox of drying and preparation method thereof - Google Patents
A kind of quick Ludox of drying and preparation method thereof Download PDFInfo
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- CN106365171B CN106365171B CN201610730102.8A CN201610730102A CN106365171B CN 106365171 B CN106365171 B CN 106365171B CN 201610730102 A CN201610730102 A CN 201610730102A CN 106365171 B CN106365171 B CN 106365171B
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- Prior art keywords
- ludox
- humic acid
- quick
- acid
- stirred
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000001035 drying Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004021 humic acid Substances 0.000 claims abstract description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 230000004308 accommodation Effects 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 8
- 239000004952 Polyamide Substances 0.000 claims abstract description 6
- 229920002647 polyamide Polymers 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000002585 base Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000005416 organic matter Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000002689 soil Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 7
- 229910052681 coesite Inorganic materials 0.000 abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 6
- 239000000377 silicon dioxide Substances 0.000 abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003292 glue Substances 0.000 description 5
- 239000003607 modifier Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of quick Ludox preparation methods of drying, including following S01, prepare Humic Acid Solution, between then progress acid-base accommodation makes its pH be 8 ~ 10;The Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred by S02, forms humic acid/Ludox mixed system;S03 is washed with absolute ethyl alcohol after being filtered the humic acid obtained in S02/Ludox mixed system, finally the mixture being obtained by filtration is re-dispersed into polyamide emulsion hydrosol, and dry quick Ludox is made.The quick Ludox of drying prepared by the present invention, SiO2Particle is evenly dispersed in polymer emulsion, and product is cost-effective and has the characteristic of environmental protection.
Description
Technical field
The present invention relates to quick Ludox of a kind of drying and preparation method thereof, belong to technical field of nano material.
Background technology
Ludox is dispersion liquid of the nano level silica dioxide granule in water or in solvent, has large specific surface area, resistance to
The characteristics such as high temperature, anti-oxidant are a kind of ideal polymer emulsion increasings
Strong material.Due to the Nano-meter SiO_2 in Ludox2Particle surface needs to carry out hydrophobic change to it there are great amount of hydroxy group
Property, make SiO2Particle is can be uniformly dispersed in polymer emulsion.So far, main modifying agent mainly includes machine modifying agent
With metal modifiers two major classes.Organic modifiers are mainly silane coupling agent, but silane coupling agent can occur acutely in water
Hydrolysis-condensation reaction, lead to the generation of gel;Metal modifiers are the most commonly used is aluminium, tin, zinc and lead, but metal modifiers
Cost is higher, the problems such as in addition causing heavy metal pollution.In addition, common Ludox slow drying speed, causes the production cycle
Extend, is unfavorable for the raising of production efficiency.
Invention content
The technical problem to be solved by the present invention is to provide that a kind of Ludox arid cycle is short, SiO2Uniform particle dispersion
The preparation method of dry quick Ludox;Further, it is molten to provide a kind of cost-effective, environment-friendly type quick silicon of drying by the present invention
Glue and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of quick Ludox preparation method of drying, includes the following steps:
S01 prepares Humic Acid Solution, between then progress acid-base accommodation makes its pH be 8 ~ 10;
The Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred by S02, and it is molten to form humic acid/silicon
Glue mixed system;
S03 is washed after being filtered the humic acid obtained in S02/Ludox mixed system with absolute ethyl alcohol, most
The mixture being obtained by filtration is re-dispersed into polyamide emulsion hydrosol afterwards, dry quick Ludox is made.
A concentration of 30 ~ 40wt% of the silicon sol solution.
The humic acid is extracted from the soil organism or water body organic matter.
The acid of the acid-base accommodation includes dilute hydrochloric acid or dust technology, and the alkali of the acid-base accommodation includes sodium hydroxide.
Between a concentration of 1000mg/L to the 2000mg/L of the humic acid.
Further include any one of the following conditions or multinomial in S02:
A. the reaction temperature being stirred is 40oC to 50oBetween C;
B. described to be stirred to be persistently stirred, the time being persistently stirred is at least 24 hours;
C. the drop rate of the humic acid is 5 ~ 10mL/min.
A kind of quick Ludox of drying, is made by aforementioned preparation process.
Beneficial effects of the present invention:A kind of rapid draing Ludox provided by the invention and preparation method thereof, polyamide breast
The setting of glue can shorten Ludox arid cycle, the Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred
Mixing forms humic acid/Ludox mixed system, SiO2Particle can adsorb the humic acid with negative electrical charge, make itself band
There is negative electrical charge, increases SiO2Repulsive interaction between particle, final SiO2Evenly dispersed formed is not easy particle in water or in solvent
The Ludox stability reunite, generated is high;The humic acid is extracted from the soil organism or water body organic matter, and humic acid exists
It is widely present in nature, occupies the major part in natural organic matter, select material of the humic acid as modified silicasol, at
This is relatively low, and humic acid itself is extremely stablized, will not generation environment pollution, have the effect of environmental protection.
Specific implementation mode
The knot present invention is further described below, and following embodiment is only used for clearly illustrating the technical side of the present invention
Case, and not intended to limit the protection scope of the present invention.
Embodiment 1
A kind of quick Ludox preparation method of drying, includes the following steps:
S01 prepares Humic Acid Solution, and then carrying out acid-base accommodation makes its pH be 8;
The Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred by S02, and it is molten to form humic acid/silicon
Glue mixed system;
S03 is washed after being filtered the humic acid obtained in S02/Ludox mixed system with absolute ethyl alcohol, most
The mixture being obtained by filtration is re-dispersed into polyamide emulsion hydrosol afterwards, dry quick Ludox is made.
A concentration of 30wt% of the silicon sol solution.
The humic acid is extracted from the soil organism or water body organic matter.
The acid of the acid-base accommodation includes dilute hydrochloric acid or dust technology, and the alkali of the acid-base accommodation includes sodium hydroxide.
A concentration of 1000mg/L of the humic acid.
Further include any one of the following conditions or multinomial in S02:
A. the reaction temperature being stirred is 40oC;
B. described to be stirred to be persistently stirred, at least 24 hours time being persistently stirred;
C. the drop rate of the humic acid is 5mL/min.
A kind of quick Ludox of drying, is made by aforementioned preparation process.
Embodiment 2
A kind of quick Ludox preparation method of drying, includes the following steps:
S01 prepares Humic Acid Solution, and then carrying out acid-base accommodation makes its pH be 10;
The Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred by S02, and it is molten to form humic acid/silicon
Glue mixed system;
S03 is washed after being filtered the humic acid obtained in S02/Ludox mixed system with absolute ethyl alcohol, most
The mixture being obtained by filtration is re-dispersed into polyamide emulsion hydrosol afterwards, dry quick Ludox is made.
A concentration of 40wt% of the silicon sol solution.
The humic acid is extracted from the soil organism or water body organic matter.
The acid of the acid-base accommodation includes dilute hydrochloric acid or dust technology, and the alkali of the acid-base accommodation includes sodium hydroxide.
A concentration of 2000mg/L of the humic acid.
Further include any one of the following conditions or multinomial in S02:
A. the reaction temperature being stirred is 50oC;
B. described to be stirred to be persistently stirred, at least 24 hours time being persistently stirred;
C. the drop rate of the humic acid is 10mL/min.
A kind of quick Ludox of drying, is made by aforementioned preparation process.
The above is only a preferred embodiment of the present invention, it should be pointed out that:For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (3)
1. a kind of quick Ludox preparation method of drying, it is characterised in that:Include the following steps:
S01 configures Humic Acid Solution, between then progress acid-base accommodation makes its pH be 8 ~ 10;
The Humic Acid Solution obtained in S01 is added drop-wise in silicon sol solution and is stirred by S02, and it is mixed to form humic acid/Ludox
Zoarium system;
S03 is washed after being filtered the humic acid obtained in S02/Ludox mixed system with absolute ethyl alcohol, finally will
The mixture being obtained by filtration is re-dispersed into polyamide emulsion hydrosol, and dry quick Ludox is made;
A concentration of 30 ~ 40wt% of the silicon sol solution;
Between a concentration of 1000mg/L to the 2000mg/L of the humic acid;
Further include the following conditions in S02:
A. the reaction temperature being stirred is 40oC to 50oBetween C;
B. described to be stirred to be persistently stirred, the time being persistently stirred is at least 24 hours;
C. the drop rate of the Humic Acid Solution is 5 ~ 10mL/min.
2. the quick Ludox preparation method of a kind of drying according to claim 1, it is characterised in that:The humic acid is from soil
It is extracted in earth organic matter or water body organic matter.
3. the quick Ludox preparation method of a kind of drying according to claim 1, it is characterised in that:The acid-base accommodation
Acid includes dilute hydrochloric acid or dust technology, and the alkali of the acid-base accommodation includes sodium hydroxide.
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CN201610730102.8A CN106365171B (en) | 2016-08-26 | 2016-08-26 | A kind of quick Ludox of drying and preparation method thereof |
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CN201610730102.8A CN106365171B (en) | 2016-08-26 | 2016-08-26 | A kind of quick Ludox of drying and preparation method thereof |
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CN106365171B true CN106365171B (en) | 2018-08-28 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000178020A (en) * | 1998-12-15 | 2000-06-27 | Nippon Chem Ind Co Ltd | High purity silica aqueous sol and method for producing the same |
CN1907851A (en) * | 2005-08-02 | 2007-02-07 | 日产化学工业株式会社 | Organosol of silica and process for producing the same |
CN101475180A (en) * | 2009-01-16 | 2009-07-08 | 清华大学 | Purification method of ultra-pure silicon dioxide sol |
CN104607591A (en) * | 2015-01-16 | 2015-05-13 | 青岛新诺科铸造材料科技有限公司 | Quick-drying silica sol and preparation method thereof |
-
2016
- 2016-08-26 CN CN201610730102.8A patent/CN106365171B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000178020A (en) * | 1998-12-15 | 2000-06-27 | Nippon Chem Ind Co Ltd | High purity silica aqueous sol and method for producing the same |
CN1907851A (en) * | 2005-08-02 | 2007-02-07 | 日产化学工业株式会社 | Organosol of silica and process for producing the same |
CN101475180A (en) * | 2009-01-16 | 2009-07-08 | 清华大学 | Purification method of ultra-pure silicon dioxide sol |
CN104607591A (en) * | 2015-01-16 | 2015-05-13 | 青岛新诺科铸造材料科技有限公司 | Quick-drying silica sol and preparation method thereof |
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