CN102382488B - Method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings - Google Patents
Method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings Download PDFInfo
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- CN102382488B CN102382488B CN 201010267034 CN201010267034A CN102382488B CN 102382488 B CN102382488 B CN 102382488B CN 201010267034 CN201010267034 CN 201010267034 CN 201010267034 A CN201010267034 A CN 201010267034A CN 102382488 B CN102382488 B CN 102382488B
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- Prior art keywords
- wollastonite
- type composite
- fillings
- antistatic function
- loaded
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- 239000010456 wollastonite Substances 0.000 title claims abstract description 36
- 229910052882 wollastonite Inorganic materials 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title abstract description 14
- 238000000034 method Methods 0.000 title abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000000376 reactant Substances 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 6
- 238000004537 pulping Methods 0.000 claims abstract description 4
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 7
- 230000001143 conditioned effect Effects 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000004033 plastic Substances 0.000 abstract description 4
- 229920003023 plastic Polymers 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 230000000638 stimulation Effects 0.000 abstract 1
- 239000002216 antistatic agent Substances 0.000 description 9
- 239000000945 filler Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011175 product filtration Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
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Abstract
The invention relates to a method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings. Water is added into wollastonite to carry out stirring and pulping, and SnCl4 solution is added for carrying out hydrolysis reaction; ammonia water is used for regulating the pH of reactants; after the reactants are raised to a certain temperature, the temperature is maintained, and the reaction lasts a period of time; and finally, the reactants are filtered, washed, dried and calcined, and the wollastonite loaded nanometer SnO2 type composite antistatic function fillings are obtained. The wollastonite loaded nanometer SnO2 type composite antistatic function fillings have the advantages that no toxicity and no stimulation exist, the whiteness is high, the price is low, the original advantages of the wollastonite used as the fillings are reserved, in addition, the resistivity of the wollastonite is obviously reduced, and the wollastonite loaded nanometer SnO2 type composite antistatic function fillings can be widely used as antistatic fillings of materials such as plastics, rubber products, chemical fibers and the like.
Description
1. technical field
The present invention relates to a kind of wollastonite loaded with nano SnO
2The preparation method of type composite anti-static functional stuffing belongs to mineral processing and mineral material field.
2. background technology
Antistatic material is that a kind of industry and civil use material and device of preventing produces the general name of a class material of static.Each industrially developed country of the world all attaches great importance to Antistatic Materials, production and use, particularly at some specific area, all generally use antistatic material as electronic computer room floor, particular packing and Turnover Box, industrial packaging film, mine with tubing etc.Used static inhibitor to become the main means of antistatic technology since oneth century, still for many industrial circles, static hazard still is problem demanding prompt solution.As at field of plastics processing, thermoplastic engineering plastic processing temperature height, processing conditions are very harsh, press for exploitation good stability, the better antistatic material of processed-type; In addition, in textile industry, the anti-quiet filler that requires to have high thermal stability and better static resistance and practicality arranged is in order to prepare the melt-spinning synthon.
The inorganic antistatic material is that a kind of use temperature is higher, the antistatic material of stable performance.In engineering materials, use more inorganic antistatic material or filler at present based on graphite, carbon black, metal oxide etc.It mainly is to utilize methods such as physics, chemistry, and interpolation or filling graphite, carbon black, metal oxide etc. are to reach anlistatig purpose in product.But graphite and carbon black color are dark, and the product colour of producing is malleable not, and it is attractive in appearance to influence product, has limited the range of application of product; It is higher and can influence the performance such as mechanics, calorifics of product to add single metal oxide production cost.Therefore, need the novel inorganic antistatic material that the exploitation use properties is better, whiteness is high and production cost is lower.
The wollastonite whiteness is higher, and raw material sources are extensive, and tooling cost is lower, and has the raphioid fiber structure, and good strengthening and toughening performance is arranged, and has been widely used as the strengthening and toughening filler of plastics etc.Therefore, the objective of the invention is shortcoming or deficiency at existing inorganic antistatic material, propose a kind of be carrier with the wollastonite, with SnCl
45H
2O is the tindioxide presoma, adopts the neutralizing hydrolysis precipitator method at wollastonite particle surface loaded with nano SnO
2, prepare and have the good resistance antistatic property and fill the wollastonite composite anti-static functional stuffing strengthen the property.
3. summary of the invention
Wollastonite is added the water stirring pulping, add SnCl
4The solution reaction that is hydrolyzed; PH with ammoniacal liquor conditioned reaction thing; Reactant is risen to insulation reaction certain hour after the certain temperature; With reactant filtration, washing, dry and calcining, namely get wollastonite loaded with nano SnO at last
2Type composite anti-static functional stuffing.
SnCl
4Hydrolysis reaction generates tindioxide to carry out in two steps, and its reactive chemistry equation is as follows:
SnCl
4+4OH
-＝Sn(OH)
4+4Cl
-
Sn(OH)
4＝SnO
2↓+2H
2O
Its step of preparation process is as follows:
(1) the wollastonite pulp preparation adds wollastonite the water stirring pulping and is adjusted to finite concentration;
(2) nano SnO
2Load is lowered the temperature to slurry, treats that adding the certain density tin tetrachloride aqueous solution after temperature is down to below 5 ℃ carries out stirring reaction; The pH that adds ammoniacal liquor conditioned reaction thing; Insulation reaction 10～120min after then reactant being warmed up to 10～100 ℃;
(3) with the filtration of step (2) reactant, washing, dry and calcining.
Below be prescription of the present invention and main technique condition:
(1) mass concentration of wollastonite pulp preparation wollastonite slurries is 5%～20%.
(2) nano SnO
2Loaded with nano SnO
2Covering amount (mass percent) is 0.2%～10%; Reaction end pH value is 3～9.
(3) reactant filtration, washing, drying and calcining drying temperature are 90～120 ℃; 200～1000 ℃ of calcining temperatures, soaking time 0.5～8h.
Be further elaborated below by the present invention of embodiment, protection scope of the present invention is not limited by the cases cited.
Wollastonite loaded with nano SnO with the present invention's preparation
2Type composite anti-static functional stuffing is nontoxic, non-stimulated, whiteness is high, inexpensive, not only kept the original advantage as filler of wollastonite, and significantly reduced the resistivity of wollastonite, can extensively be used as the antistatic filler of materials such as plastics, rubber item, chemical fibre.
4. accompanying drawing content
Accompanying drawing is process flow sheet of the present invention.
5. embodiment
Embodiment one:
Get wollastonite 30g, in reactor, add water 210mL, dispersed with stirring and to be cooled to adding prepares after 5 ℃ concentration be that the tin tetrachloride aqueous solution 8mL of 0.4mol/L stirs that to add ammoniacal liquor conditioned reaction liquid pH value be 7 in the back; Stirring reaction also is warming up to 20 ℃, reacts 50min then under 20 ℃ of temperature; 6h is calcined in reaction product filtration, the insulation under 800 ℃ of dry back, namely get wollastonite loaded with nano SnO
2The type composite powder material.
Embodiment two:
Get wollastonite 30g, in reactor, add water 270mL, dispersed with stirring and to be cooled to adding prepares after 5 ℃ concentration be that the tin tetrachloride aqueous solution 2mL of 0.4mol/L stirs that to add ammoniacal liquor conditioned reaction liquid pH value be 6 in the back; Stirring reaction also is warming up to 60 ℃, reacts 40min then under 60 ℃ of temperature; 4h is calcined in reaction product filtration, the insulation under 1000 ℃ of dry back, namely get wollastonite loaded with nano SnO
2The type composite powder material.
Embodiment three:
Get wollastonite 30g, in reactor, add water 310mL, dispersed with stirring and to be cooled to adding prepares after 5 ℃ concentration be that the tin tetrachloride aqueous solution 6mL of 0.4mol/L stirs that to add ammoniacal liquor conditioned reaction liquid pH value be 5 in the back; Stirring reaction also is warming up to 80 ℃, reacts 30min then under 80 ℃ of temperature; 5h is calcined in reaction product filtration, the insulation under 900 ℃ of dry back, namely get wollastonite loaded with nano SnO
2The type composite powder material.
Table 1 is the embodiment test result of samples.
The detection analytical results of table 1 embodiment sample
| Embodiment | SnO 2Charge capacity/%w | Resistivity [1]/kΩ·cm |
| Wollastonite | 0 | 10.683 |
| 1 | 1.6 | 3.8888 |
| 2 | 0.4 | 2.5326 |
| 3 | 1.2 | 2.9526 |
Annotate: [1] is pressed into the thin slice of diameter 50mm, thickness 2mm with the 5g composite granule, with four point probe resistivity tester test gained result.
Claims (2)
1. wollastonite loaded with nano SnO
2The preparation method of type composite anti-static functional stuffing is characterized in that its step of preparation process is:
1. wollastonite pulp preparation: wollastonite is added the water stirring pulping, and the mass concentration of wollastonite slurry is adjusted to 5%～20%;
2. nano SnO
2Load: slurry is lowered the temperature, treat that temperature is down to below 5 ℃ the back by wollastonite surface SnO
2The tin tetrachloride aqueous solution that coats quality 0.2%～10% adding respective quality carries out stirring reaction; The endpoint pH that adds ammoniacal liquor conditioned reaction thing is 3～9; Insulation reaction 10～120min after then reactant being warmed up to 10～100 ℃;
3. with 2. reactant filtration of step, washing, dry and calcining.
2. wollastonite loaded with nano SnO according to claim 1
2The preparation method of type composite anti-static functional stuffing, it is characterized in that described with reactant filter, washing, dry and calcining, its processing condition are: 90～120 ℃ of drying temperatures; 200～1000 ℃ of calcining temperatures, soaking time 0.5～8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010267034 CN102382488B (en) | 2010-08-31 | 2010-08-31 | Method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010267034 CN102382488B (en) | 2010-08-31 | 2010-08-31 | Method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102382488A CN102382488A (en) | 2012-03-21 |
| CN102382488B true CN102382488B (en) | 2013-07-10 |
Family
ID=45822351
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010267034 Active CN102382488B (en) | 2010-08-31 | 2010-08-31 | Method for preparing wollastonite loaded nanometer SnO2 type composite antistatic function fillings |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102382488B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6395149B1 (en) * | 1998-06-30 | 2002-05-28 | 3M Innovative Properties Company | Method of making light colored, electrically conductive coated particles |
| CN1462775A (en) * | 2003-05-27 | 2003-12-24 | 中国地质大学（武汉） | Method for modifying wollastonite |
| CN101724175A (en) * | 2008-10-15 | 2010-06-09 | 中国矿业大学(北京) | Inorganic compounding and surface modifying method of wollastonite stuffing |
-
2010
- 2010-08-31 CN CN 201010267034 patent/CN102382488B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6395149B1 (en) * | 1998-06-30 | 2002-05-28 | 3M Innovative Properties Company | Method of making light colored, electrically conductive coated particles |
| CN1462775A (en) * | 2003-05-27 | 2003-12-24 | 中国地质大学（武汉） | Method for modifying wollastonite |
| CN101724175A (en) * | 2008-10-15 | 2010-06-09 | 中国矿业大学(北京) | Inorganic compounding and surface modifying method of wollastonite stuffing |
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| Publication number | Publication date |
|---|---|
| CN102382488A (en) | 2012-03-21 |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191008 Address after: 100083 Beijing City, Haidian District Institute of Rutosids No. 11 Co-patentee after: Xinyu Nanfang wollastonite Co., Ltd. Patentee after: China University of Mining and Technology (Beijing) Address before: 100083 Beijing City, Haidian District Institute of Rutosids No. 11 Patentee before: China University of Mining and Technology (Beijing) |
|
| TR01 | Transfer of patent right |