Lanthanum oxide-silicon dioxide composite particulate material and preparation method thereof

Abstract

The invention which relates to a lanthana-silica composite particulate material and a preparation method thereof belongs to the technical field of rare earth oxide-white carbon black composite particulate materials. The lanthana-silica composite particulate material is characterized in that a general formula of the lanthana-silica composite particulate material is (SiO2)x.(La2O3)1-x, and x is equal to or more than 0.4 and equal to or less than 0.99. The preparation method is characterized in that the lanthana-silica composite particulate material is obtained by simultaneously adding a sulfuric acid solution and a soluble inorganic lanthanum salt liquid to an alkaline sodium silicate solution with certain concentration drop by drop by a metering pump according to a preset flow ratio to precipitate silica and a sediment containing lanthanum from a solution to form a composite sediment, aging, washing, and drying. The lanthana-silica composite particulate material of the present invention which integrates characteristics of rare earths and white carbon blacks allows the processability, the mechanical performances and the chemical performances of rubber materials to be improved, the rare earth assistant to be nontoxic and harmless, and the consumption of the rare earth assistant to be less.

Description

Technical field:

[0001] The invention relates to a white carbon black reinforcing material used in the rubber industry, in particular to a preparation method of a lanthanum oxide-white carbon black composite particulate material. Background technique:

[0002] Among the components of rubber, besides raw rubber, the most used one is the reinforcing material. It can not only improve the physical and mechanical properties of rubber products, but also improve the processing performance of rubber materials to a certain extent, and can reduce the cost of products.

[0003] There are many types of reinforcing agents, and the most used ones are carbon black and silica. Carbon black can give tires good reinforcement performance. Silica is an important substitute for carbon black. As a reinforcing material, it is used for The production of green tires can significantly increase the tear strength and crack growth resistance of the sidewall without significantly affecting the vulcaniza...

Examples

preparation example Construction

[0033] The preparation of the sodium silicate solution in the step A adopts reagent Na 2 SiO 3 9H 2O; Soluble lanthanum inorganic salt can be lanthanum nitrate, lanthanum chloride, lanthanum sulfate, and what lanthanum nitrate adopts is La(NO 3 ) 3 , lanthanum chloride uses LaCl 3 ·7H 2 O, lanthanum sulfate is La 2 (SO 4 ) 3 ·8H 2 O; concentrated sulfuric acid is the concentrated sulfuric acid that mass percent is 98%; The water of preparation solution adopts deionized water.

[0034] The preparation of lanthanum oxide-silicon dioxide composite particulate material by adopting three kinds of soluble lanthanum inorganic salts of lanthanum chloride, lanthanum sulfate and lanthanum nitrate in the present invention is explained respectively below:

[0035] Table 1. Using sodium silicate and lanthanum nitrate as raw materials

[0036]

[0037] Table 2. Process parameters in embodiments 1-4

[0038]

[0039] Table 3. Using sodium silicate and lanthanum chloride as r...

Embodiment 1

[0051] A. Weigh 21.3g Na 2 SiO 3 9H 2 O, dissolved in 50mL deionized water to prepare a 1.5M aqueous solution, dissolved in a water bath, and set the temperature of the water bath to 90°C; weigh 14.3g of lanthanum nitrate and dissolve it in 15mL deionized water to prepare a 3.0M aqueous solution, weighing Take 7.5g of concentrated sulfuric acid and slowly add it into water, dilute to 14.7g of sulfuric acid solution with a mass concentration of 50%;

[0052] B. When the temperature of the sodium silicate solution reaches 25°C, start to add sulfuric acid solution and lanthanum nitrate solution dropwise while stirring. 1:1;

[0053] C. When the pH value of the reaction solution was about 2, stop adding the sulfuric acid solution dropwise, and the temperature of the reaction solution was heated to 90°C;

[0054] D. Adjust the pH value to 4 with ammonia water with a volume ratio of 1:1, age for 1 hour, and control the temperature at 90°C;

[0055] E. Adjust the pH value to 7, ...

Embodiment 13

[0058] A. Weigh 56.8g Na 2 SiO 3 9H 2 O, dissolved in 100mL deionized water to prepare a 2.0M aqueous solution, dissolved in a water bath, set the water bath temperature to 70°C; weighed 2.27g of lanthanum nitrate dissolved in 7mL deionized water to prepare a 1M aqueous solution, weighed Slowly add 20g of concentrated sulfuric acid into water, dilute to 78.4g of sulfuric acid solution with a mass concentration of 25%;

[0059] B. When the temperature of the sodium silicate solution reaches 40°C, start to add sulfuric acid solution and lanthanum nitrate solution dropwise while stirring. 10:1;

[0060] C. When the pH value of the reaction solution was about 2, stop adding the sulfuric acid solution dropwise, and the temperature of the reaction solution was heated to 70°C;

[0061] D. Adjust the pH value to 4 with ammonia water with a volume ratio of 1:1, age for 1 hour, and control the temperature at 70°C;

[0062] E. Adjust the pH value to 7, filter, wash and dry.

[0063...

Technical field:

[0001] The invention relates to a white carbon black reinforcing material used in the rubber industry, in particular to a preparation method of a lanthanum oxide-white carbon black composite particulate material. Background technique:

[0002] Among the components of rubber, besides raw rubber, the most used one is the reinforcing material. It can not only improve the physical and mechanical properties of rubber products, but also improve the processing performance of rubber materials to a certain extent, and can reduce the cost of products.

[0003] There are many types of reinforcing agents, and the most used ones are carbon black and silica. Carbon black can give tires good reinforcement performance. Silica is an important substitute for carbon black. As a reinforcing material, it is used for The production of green tires can significantly increase the tear strength and crack growth resistance of the sidewall without significantly affecting the vulcaniza...

Examples

preparation example Construction

[0033] The preparation of the sodium silicate solution in the step A adopts reagent Na 2 SiO 3 9H 2O; Soluble lanthanum inorganic salt can be lanthanum nitrate, lanthanum chloride, lanthanum sulfate, and what lanthanum nitrate adopts is La(NO 3 ) 3 , lanthanum chloride uses LaCl 3 ·7H 2 O, lanthanum sulfate is La 2 (SO 4 ) 3 ·8H 2 O; concentrated sulfuric acid is the concentrated sulfuric acid that mass percent is 98%; The water of preparation solution adopts deionized water.

[0034] The preparation of lanthanum oxide-silicon dioxide composite particulate material by adopting three kinds of soluble lanthanum inorganic salts of lanthanum chloride, lanthanum sulfate and lanthanum nitrate in the present invention is explained respectively below:

[0035] Table 1. Using sodium silicate and lanthanum nitrate as raw materials

[0036]

[0037] Table 2. Process parameters in embodiments 1-4

[0038]

[0039] Table 3. Using sodium silicate and lanthanum chloride as r...

Embodiment 1

[0051] A. Weigh 21.3g Na 2 SiO 3 9H 2 O, dissolved in 50mL deionized water to prepare a 1.5M aqueous solution, dissolved in a water bath, and set the temperature of the water bath to 90°C; weigh 14.3g of lanthanum nitrate and dissolve it in 15mL deionized water to prepare a 3.0M aqueous solution, weighing Take 7.5g of concentrated sulfuric acid and slowly add it into water, dilute to 14.7g of sulfuric acid solution with a mass concentration of 50%;

[0052] B. When the temperature of the sodium silicate solution reaches 25°C, start to add sulfuric acid solution and lanthanum nitrate solution dropwise while stirring. 1:1;

[0053] C. When the pH value of the reaction solution was about 2, stop adding the sulfuric acid solution dropwise, and the temperature of the reaction solution was heated to 90°C;

[0054] D. Adjust the pH value to 4 with ammonia water with a volume ratio of 1:1, age for 1 hour, and control the temperature at 90°C;

[0055] E. Adjust the pH value to 7, ...

Embodiment 13

[0058] A. Weigh 56.8g Na 2 SiO 3 9H 2 O, dissolved in 100mL deionized water to prepare a 2.0M aqueous solution, dissolved in a water bath, set the water bath temperature to 70°C; weighed 2.27g of lanthanum nitrate dissolved in 7mL deionized water to prepare a 1M aqueous solution, weighed Slowly add 20g of concentrated sulfuric acid into water, dilute to 78.4g of sulfuric acid solution with a mass concentration of 25%;

[0059] B. When the temperature of the sodium silicate solution reaches 40°C, start to add sulfuric acid solution and lanthanum nitrate solution dropwise while stirring. 10:1;

[0060] C. When the pH value of the reaction solution was about 2, stop adding the sulfuric acid solution dropwise, and the temperature of the reaction solution was heated to 70°C;

[0061] D. Adjust the pH value to 4 with ammonia water with a volume ratio of 1:1, age for 1 hour, and control the temperature at 70°C;

[0062] E. Adjust the pH value to 7, filter, wash and dry.

[0063...

Images