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Antimonic oxide sol and method for its preparation

A technology of antimony pentoxide and antimony trioxide, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxoacid, inorganic chemistry, etc., can solve the problems of less easy oxidation, lower sol refractive index, Problems such as yellow color of antimony pentoxide sol

Active Publication Date: 2007-11-28
NISSAN CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this reaction carried out in the presence of an inorganic alkaline substance has the disadvantage of causing the resulting antimony pentoxide sol to have a more yellowish color, and there are certain limitations when it is used as a microfiller for a coating agent.
[0012] In addition, the silicon oxide / antimony oxide composite sol prepared under the condition of the presence of inorganic silicon compounds contains silicon oxide in its composition, and has the disadvantage that the refractive index of the sol itself decreases
[0013] For the conventional oxidation method described above, even if the reaction occurs in, for example, H 2 o 2 / Sb 2 o 3 It is not easy to oxidize Sb(III) to Sb when the molar ratio is 3.0 (that is, an excess of 2.0). 2 o 3 / Sb 2 o 5 The weight ratio is up to 5%, and due to the residual Sb (III), a part of the product is in an intermediate oxidation state, and the yellow color of the resulting sol will become more and more intense (the yellow index (YI value) is high), so that the sol is used for transparency There are limitations when coating materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] In a 2-liter reaction flask equipped with a stirrer, dissolve 10.42 g (in WO 3 Calculated as 7.20g) sodium tungstate dihydrate (Na 2 WO 4 2H 2 O, manufactured by Kisan Kinzoku Chemicals Co., Ltd., as WO 3 Containing 69.1% by weight), then, 130.4g antimony trioxide (Sb 2 o 3 , content 99.5% by weight, manufactured by Guangdong Mikuni Antimony Industries Co., Ltd) was dispersed in, and 86.6 g of 35% by weight aqueous hydrogen peroxide solution was added, and the mixture was heated to react at this time. h 2 o 2 / Sb 2 o 3 The molar ratio is 2.0, WO 3 / Sb 2 o 3 The weight ratio is 5.5% by weight.

[0049] During the reaction, the temperature of the liquid was 85-90°C. After completing the above, stirring was continued at 90° C. for 1 hour to obtain 1906 g of a slightly yellowish white sol. The primary particle size of the resulting sol is 15-25 nm, the pH is 2.50, the conductivity is 575 μs / cm, and the Sb 2 o 5 The content is 7.28% by weight, Sb 2 o 3 The ...

Embodiment 2

[0051] In a 2-liter reaction flask equipped with a stirrer, dissolve 10.42 g (in WO 3 Calculated as 7.20g) sodium tungstate dihydrate (Na 2 WO 4 2H 2 O, manufactured by Kisan Kinzoku Chemicals Co., Ltd., as WO 3 Containing 69.1% by weight), then, 130.4g antimony trioxide (Sb 2 o 3 , content 99.5% by weight, manufactured by Guangdong Mikuni Antimony Industries Co., Ltd) dispersed in, then added 5.14g of 85% by weight of phosphoric acid aqueous solution and 86.6g of 35% by weight of hydrogen peroxide solution, at this time the mixture was heated to make reaction. h 2 o 2 / Sb 2 o 3 The molar ratio is 2.0, WO 3 / Sb 2 o 3 The weight ratio is 5.5% by weight, P 2 o 5 / Sb 2 o 3 The weight ratio is 2.4% by weight.

[0052] During the reaction, the temperature of the liquid was 85-90°C. After completion of the reaction, stirring was continued at 90° C. for 1 hour to obtain 1903 g of a slightly yellowish sol. The primary particle size of the obtained sol is 8-15 nanome...

Embodiment 3

[0054] In a 1-liter reaction flask equipped with a stirrer, dissolve 1.94 g (as WO 3 Calculated as 1.34g) sodium tungstate dihydrate (Na 2 WO 4 2H 2 O, manufactured by Kisan Kinzoku Chemicals Co., Ltd., as WO 3 Contains 69.1% by weight), then, 60.68g antimony trioxide (Sb 2 o 3 , content 99.5% by weight, manufactured by Guangdong Mikuni Antimony Industries Co., Ltd) dispersed in, then added 52.39g of 85% by weight of phosphoric acid aqueous solution and 40.27g of 35% by weight of hydrogen peroxide solution, at this time the mixture was heated to make reaction. h 2 o 2 / Sb 2 o 3 The molar ratio is 2.0, WO 3 / Sb 2 o 3 The weight ratio is 2.2% by weight, P 2 o 5 / Sb 2 o 3 The weight ratio is 2.4% by weight.

[0055] During the reaction, the temperature of the liquid was 85-90°C. After the reaction was completed, stirring was continued at 90° C. for 1 hour to obtain 886.5 g of a slightly yellowish sol. The primary particle size of the obtained sol is 8-15 nanome...

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Abstract

A sol comprising diantimony pentoxide particles having a primary particle size of from 2 to 50 nm and a Sb2O3 / Sb2O5 weight ratio of at most 4 wt%.

Description

technical field [0001] The invention relates to a method for preparing antimony pentoxide sol with high oxidation purity. technical background [0002] Antimony pentoxide sol can be used as a flame retardant additive for plastics, fibers, etc., as a microfiller for surface treatment agents for plastics or glass, as an inorganic ion exchanger, as a catalyst component, as a pigment component, etc. Typically, high concentration sols (containing 30-50% by weight Sb) stabilized by organic bases are used 2 o 5 ). [0003] Hitherto, antimony pentoxide sols have been produced by the following known methods. [0004] That is, the method of removing alkali metal antimonate ions by cation exchange resin (JP-A-52-21298, U.S.P.4,110,247, JP-B-57-11848), after the reaction of alkali metal antimonate and inorganic acid Followed by the method of peptization (JP-A-60-41536, JP-A-61-227918) and the like. [0005] As a method other than the above, a method of oxidizing antimony trioxide w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00C09C1/00C09K21/02
CPCC09C1/0096C01G30/005C09K21/02C01P2004/61
Inventor 铃木启太郎小山欣也
Owner NISSAN CHEM CORP