CN114291879B - A kind of preparation method of aluminum silicate - Google Patents

Abstract

The invention relates to the field of chemical industry and discloses a preparation method of aluminum silicate. The method comprises the following steps: (1) Adding aluminum sulfate into the silicon-containing alkaline vanadium liquid, reacting under stirring, and then filtering and washing to obtain precipitation slag; (2) Adding the precipitate slag obtained in the step (1) into water for pulping, then adding glucose for reaction, then adding ethanol for reaction, and then filtering, washing and drying; wherein the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium solution is 1:2.8-3. The sodium vanadate solution obtained after water leaching in the vanadium slag sodium roasting-water leaching vanadium extraction process is treated by the method, and the high-purity aluminum silicate product can be obtained on the premise of ensuring high-efficiency removal of impurity silicon, so that the emission of waste is reduced, and the recycling is realized. The obtained high-purity aluminum silicate product can be directly used as a raw material for producing pigments and coatings.

Description

A kind of preparation method of aluminum silicate

technical field

The invention relates to the field of chemical industry, in particular to a method for preparing aluminum silicate.

Background technique

Vanadium slag sodium roasting-water leaching vanadium extraction process, mainly uses sodium salt as roasting additive, roasts under high temperature and aerobic conditions, generates sodium vanadate soluble in water, obtains sodium vanadate solution after water immersion, and further precipitates vanadium to obtain Vanadium products, but the vanadium slag contains a lot of silicon, which forms sodium silicate with sodium, and enters the solution together. If the sodium silicate is not removed in the vanadium liquid, it will affect the quality of vanadium precipitation and vanadium products.

There are many commonly used silicon removal methods. For example, it is reported in "Research on Silicon Removal by Alkaline Vanadium Liquid Precipitation" that magnesium sulfate has the best effect on silicon removal. In the "Study on Deep Impurity Removal Process of Salt-Free Roasting Leach Liquor", it is studied that quicklime is added to remove phosphorus first, and aluminum hydroxide is selected as the silicon removal agent. The impurity elements meet the requirements of the national standard. At present, a large number of literature and patent reports are still on the simple removal of silicon and phosphorus, and the obtained slag needs to be extracted twice or directly stored with the residue, and used as waste, resulting in a waste of resources.

Contents of the invention

The purpose of the present invention is to provide a kind of aluminosilicate to overcome the existing problems in the prior art that the impurity-removing slag obtained by removing silicon is stored as waste, causing waste of resources, polluting the environment, and the purity of aluminum silicate obtained by removing silicon is not high. A preparation method, the method can obtain high-purity aluminum silicate while effectively removing silicon.

In order to achieve the above object, the invention provides a kind of preparation method of aluminum silicate, described method comprises the following steps:

(1) adding aluminum sulfate to silicon-containing alkaline vanadium liquid, reacting under stirring, then filtering and washing to obtain precipitated slag;

(2) adding the precipitated slag obtained in step (1) into water for beating, then adding glucose for reaction, then adding ethanol for reaction, then filtering, washing and drying;

Wherein, the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium solution is 1:2-3.

Preferably, in step (1), the silicon concentration in the silicon-containing alkaline vanadium liquid is 0.6-3 g/L, and the pH value of the silicon-containing alkaline vanadium liquid is 9.5-10.5.

Preferably, in step (1), the reaction temperature is 95°C-99°C, and the reaction time is 30-60min.

Preferably, the specific process of the step (2) includes: adding the precipitated slag obtained in the step (1) into water for beating at 95-99° C., then adding glucose at 95-99° C. for heat preservation reaction, and then cooling to 45-99° C. Add ethanol at 60°C for heat preservation reaction, then filter, wash and dry.

Preferably, in step (2), the solid-to-liquid ratio of the precipitated slag and water is 1g:1.5-2.5mL.

Preferably, in step (2), the weight ratio of the glucose to the sediment residue is 0.3-0.5:100.

Preferably, in step (2), the amount of ethanol added is 0.05-0.3% by volume of the volume of the solution obtained by adding glucose for reaction.

Preferably, in step (2), the reaction time of adding glucose and incubating the reaction is 80-180min.

Preferably, in step (2), the reaction time of adding ethanol and insulated reaction is 30-60min.

Preferably, in step (2), the beating time is 30-45min.

By using the method of the present invention to treat the sodium vanadate solution obtained after water immersion in the vanadium slag sodium roasting-water leaching vanadium extraction process, high-purity silicon can also be obtained under the premise of ensuring efficient removal of impurity silicon Acid aluminum products reduce waste emissions and realize resource utilization. The obtained high-purity aluminum silicate products can be directly used as raw materials for the production of pigments and coatings.

Detailed ways

Specific embodiments of the present invention will be described in detail below. It should be understood that the specific embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.

Neither the endpoints nor any values of the ranges disclosed herein are limited to such precise ranges or values, and these ranges or values are understood to include values approaching these ranges or values. For numerical ranges, between the endpoints of each range, between the endpoints of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, these values Ranges should be considered as specifically disclosed herein.

The invention provides a kind of preparation method of aluminum silicate, described method comprises the following steps:

(1) adding aluminum sulfate to silicon-containing alkaline vanadium liquid, reacting under stirring, then filtering and washing to obtain precipitated slag;

(2) adding the precipitated slag obtained in step (1) into water for beating, then adding glucose for reaction, then adding ethanol for reaction, then filtering, washing and drying;

Wherein, the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium solution is 1:2-3.

In the present invention, in step (1), the silicon-containing alkaline vanadium solution may be sodium vanadate solution obtained after water immersion in the vanadium slag sodium roasting-water leaching vanadium extraction process.

In a preferred embodiment, in step (1), the concentration of silicon in the silicon-containing alkaline vanadium liquid is 0.6-3 g/L, and the pH value of the silicon-containing alkaline vanadium liquid is 9.5-10.5.

Further preferably, the concentration of vanadium in the silicon-containing alkaline vanadium liquid is 10-60 g/L.

In a preferred embodiment, in step (1), the reaction temperature is 95°C-99°C, and the reaction time is 30-60min. Specifically, the reaction temperature may be 95°C, 95.5°C, 96°C, 96.5°C, 97°C, 97.5°C, 98°C, 98.5°C or 99°C.

In a preferred embodiment, the specific process of the step (2) includes: adding the precipitated slag obtained in the step (1) into water for beating at 95-99°C, then adding glucose at 95-99°C for heat preservation reaction, and then When the temperature is lowered to 45-60°C, ethanol is added to carry out the heat preservation reaction, and then filtering, washing and drying are carried out. In a specific embodiment, the beating temperature can be 95°C, 95.5°C, 96°C, 96.5°C, 97°C, 97.5°C, 98°C, 98.5°C or 99°C; It can be 95°C, 95.5°C, 96°C, 96.5°C, 97°C, 97.5°C, 98°C, 98.5°C or 99°C; °C, 49°C, 50°C, 51°C, 52°C, 53°C, 54°C, 55°C, 56°C, 57°C, 58°C, 59°C or 60°C.

In the present invention, the precipitated slag obtained through washing in step (1) is directly used in step (2), therefore, the weight of the precipitated slag described in step (2) in the present invention is the wet weight of the precipitated slag.

In a preferred embodiment, in step (2), the solid-to-liquid ratio of the precipitated slag and water is 1g:1.5-2.5mL. Specifically, the solid-to-liquid ratio of the sediment residue and water can be 1g:1.5mL, 1g:1.6mL, 1g:1.7mL, 1g:1.8mL, 1g:1.9mL, 1g:2mL, 1g:2.1mL, 1g : 2.2mL, 1g: 2.3mL, 1g: 2.4mL or 1g: 2.5mL.

In a preferred embodiment, in step (2), the weight ratio of the glucose to the sediment residue is 0.3-0.5:100. Specifically, the weight ratio of the glucose to the sediment residue may be 0.3:100, 0.35:100, 0.4:100, 0.45:100 or 0.5:100.

In a preferred embodiment, in step (2), the amount of ethanol added is 0.05-0.3% by volume of the volume of the solution obtained by adding glucose for reaction.

In a preferred embodiment, in step (2), the reaction time of adding glucose and incubating the reaction is 80-180min. Specifically, it may be 80 min, 90 min, 100 min, 110 min, 120 min, 130 min, 140 min, 150 min, 160 min, 170 min or 180 min.

In a preferred embodiment, in step (2), the reaction time of adding ethanol and insulated reaction is 30-60min. Specifically, it may be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min or 60 min.

In a preferred embodiment, in step (2), the beating time is 30-45min. Specifically, it can be 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min or 45min.

In a preferred embodiment, in step (2), hot water is used for washing. More preferably, the temperature of the hot water is 80-95°C.

The present invention will be described in detail through examples below, but the protection scope of the present invention is not limited thereto.

The silicon-containing alkaline vanadium solution used in the following examples and comparative examples is the sodium vanadate solution obtained after water leaching in the vanadium slag sodium roasting-water leaching vanadium extraction process.

Example 1

(1) Add aluminum sulfate to silicon-containing alkaline vanadium liquid (pH=9.5, Si concentration is 0.6g/L, vanadium concentration is 10g/L), the mol ratio of aluminum sulfate and Si in silicon-containing alkaline vanadium liquid is: 1:3, stirred and reacted at 95°C for 30 minutes, then filtered and washed to obtain precipitated residue;

(2) Add the precipitated slag gained in step (1) into water and beat for 30 minutes at 95°C. The solid-to-liquid ratio of the wet weight of the precipitated slag to water is 1g:1.5mL, then add glucose (glucose and the wet weight of the precipitated slag) at 95°C The ratio is 0.3:100) heat preservation reaction 80min, add ethanol heat preservation reaction 30min when naturally cooling down to 45 ℃, ethanol addition is 0.05 volume % of the solution volume that adds glucose and carries out heat preservation reaction to obtain, then filter, hot water washing and drying.

Example 2

(1) Add aluminum sulfate to silicon-containing alkaline vanadium liquid (pH=10, Si concentration is 1.6g/L, vanadium concentration is 20g/L), the mol ratio of aluminum sulfate and Si in silicon-containing alkaline vanadium liquid is 1:3, stirred and reacted at 97°C for 45 minutes, then filtered and washed to obtain precipitated residue;

(2) adding the precipitated slag gained in step (1) into water and beating at 96°C for 38min, the solid-liquid ratio of the wet weight of the precipitated slag to water was 1g:2mL, then adding glucose (the ratio of the wet weight of glucose and the wet weight of the precipitated slag) at 96°C Ratio is 0.4:100) heat preservation reaction 140min, add ethanol heat preservation reaction 45min when naturally cooling down to 50 ℃, ethanol addition is 0.18 volume % of the solution volume that adds glucose and carries out heat preservation reaction to obtain, carry out filtration, hot water washing and drying then Dry.

Example 3

(1) Add aluminum sulfate to silicon-containing alkaline vanadium liquid (pH=10, Si concentration is 3g/L, vanadium concentration is 25g/L), the mol ratio of aluminum sulfate and Si in silicon-containing alkaline vanadium liquid is 1 : 3, stirring and reacting at 98° C. for 60 min, then filtering and washing to obtain precipitated slag;

(2) Add the precipitated slag gained in step (1) into water and beat for 45 minutes at 98°C. The solid-to-liquid ratio of the wet weight of the precipitated slag to water is 1g:2.5mL, then add glucose (glucose and the wet weight of the precipitated slag) at 98°C The ratio is 0.5:100) heat preservation reaction 180min, when natural cooling is cooled to 60 ℃, add ethanol heat preservation reaction 60min, the ethanol addition is 0.3 volume % of the solution volume that adds glucose and carries out heat preservation reaction to obtain, then filter, hot water washing and drying.

Example 4

(1) Add aluminum sulfate to silicon-containing alkaline vanadium liquid (pH=9.5, Si concentration is 0.6g/L, vanadium concentration is 30/L), the mol ratio of aluminum sulfate and Si in silicon-containing alkaline vanadium liquid is 1:2.5, stirred and reacted at 95°C for 30 minutes, then filtered and washed to obtain precipitated residue;

(2) Add the precipitated slag gained in step (1) into water and beat for 30 minutes at 95°C. The solid-to-liquid ratio of the wet weight of the precipitated slag to water is 1g:1.5mL, then add glucose (glucose and the wet weight of the precipitated slag) at 95°C The ratio is 0.3:100) heat preservation reaction 80min, add ethanol heat preservation reaction 30min when naturally cooling down to 45 ℃, ethanol addition is 0.05 volume % of the solution volume that adds glucose and carries out heat preservation reaction to obtain, then filter, hot water washing and drying.

Example 5

(1) Add aluminum sulfate to silicon-containing alkaline vanadium liquid (pH=10, Si concentration is 1.6g/L, vanadium concentration is 20g/L), the mol ratio of aluminum sulfate and Si in silicon-containing alkaline vanadium liquid is 1:2, stirred and reacted at 97°C for 45 minutes, then filtered and washed to obtain precipitated residue;

(2) adding the precipitated slag gained in step (1) into water and beating at 96°C for 38min, the solid-liquid ratio of the wet weight of the precipitated slag to water was 1g:2mL, then adding glucose (the ratio of the wet weight of glucose and the wet weight of the precipitated slag) at 96°C Ratio is 0.4:100) heat preservation reaction 140min, add ethanol heat preservation reaction 45min when naturally cooling down to 50 ℃, ethanol addition is 0.18 volume % of the solution volume that adds glucose and carries out heat preservation reaction to obtain, carry out filtration, hot water washing and drying then Dry.

Comparative example 1

Implement according to the method of Example 1, the difference is that in step (1), the molar ratio of aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:3.2.

Comparative example 2

Implement according to the method of Example 1, the difference is that in step (1), the molar ratio of aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:1.8.

test case

1, the Si concentration in the filtrate that step (1) obtains in the embodiment and the comparative example is detected, and the results are as shown in table 1.

Table 1

serial number Si concentration in silicon-containing alkaline vanadium solution g/L Si concentration in filtrate g/L Example 1 0.6 0.025 Example 2 1.6 0.038 Example 3 3.0 0.15 Example 4 0.6 0.015 Example 5 1.6 0.018 Comparative example 1 0.6 0.082 Comparative example 2 0.6 0.014

2. The purity of the aluminum silicate prepared in Examples and Comparative Examples was detected, and the results are shown in Table 2.

Table 2

serial number Aluminum silicate purity/% Example 1 99.56 Example 2 99.68 Example 3 99.79 Example 4 99.62 Example 5 99.74 Comparative example 1 99.66 Comparative example 2 94.28

From the results in Table 1 and Table 2, it can be seen that the method of the present invention can effectively remove the impurity silicon in the silicon-containing alkaline vanadium liquid, and at the same time obtain high-purity aluminum silicate products.

The preferred embodiments of the present invention have been described in detail above, however, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the content disclosed in the present invention. All belong to the protection scope of the present invention.

Claims (5)

1. a preparation method of aluminum silicate, is characterized in that, described method comprises the following steps: (1) adding aluminum sulfate to silicon-containing alkaline vanadium liquid, reacting under stirring, then filtering and washing to obtain precipitated slag; (2) Add the precipitated slag obtained in step (1) into water and beat at 95-99°C, then add glucose at 95-99°C for heat preservation reaction, then add ethanol when the temperature drops to 45-60°C for heat preservation reaction, and then carry out filtering, washing and drying; Wherein, the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium liquid is 1:2-3; In step (1), the concentration of silicon in the silicon-containing alkaline vanadium liquid is 0.6-3g/L, and the pH value of the silicon-containing alkaline vanadium liquid is 9.5-10.5; In step (1), the reaction temperature is 95°C-99°C, and the reaction time is 30-60min; In step (2), the weight ratio of the glucose to the sediment residue is 0.3-0.5:100; In step (2), the amount of ethanol added is 0.05-0.3% by volume of the solution volume obtained by adding glucose for reaction. 2. the preparation method of aluminum silicate according to claim 1, is characterized in that, in step (2), the solid-to-liquid ratio of described precipitation slag and water is 1g:1.5-2.5mL. 3. the preparation method of aluminum silicate according to claim 1 is characterized in that, in step (2), the reaction time of adding glucose insulation reaction is 80-180min. 4. the preparation method of aluminum silicate according to claim 1 is characterized in that, in step (2), the reaction time of adding ethanol insulation reaction is 30-60min. 5. the preparation method of aluminum silicate according to claim 2 is characterized in that, in step (2), beating time is 30-45min.