CN110950358A - Process for co-producing white carbon black by adding silica gel crystal seeds during production of potassium fluoride by using potassium fluosilicate - Google Patents
Process for co-producing white carbon black by adding silica gel crystal seeds during production of potassium fluoride by using potassium fluosilicate Download PDFInfo
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- CN110950358A CN110950358A CN201911411389.8A CN201911411389A CN110950358A CN 110950358 A CN110950358 A CN 110950358A CN 201911411389 A CN201911411389 A CN 201911411389A CN 110950358 A CN110950358 A CN 110950358A
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- potassium
- silica gel
- carbon black
- white carbon
- fluosilicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
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- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
Abstract
The invention discloses a process for co-producing white carbon black by adding silica gel seed crystals when potassium fluoride is produced by utilizing potassium fluosilicate. Then, adding the potassium fluosilicate and the potassium hydroxide into the silica gel crystal seed in parallel under certain process conditions, and controlling the formation and precipitation of silicon dioxide particles in the alkaline hydrolysis reaction process by means of the silica gel crystal seed to obtain the white carbon black product meeting the national standard.
Description
Technical Field
The invention relates to a process for co-producing white carbon black by adding silica gel crystal seeds when potassium fluoride is produced by utilizing potassium fluosilicate.
Background
Potassium fluoride is used as a fluorinating agent for fluorine-containing medicines and agricultural chemicals, and the market demand is expanding in recent years. In general, the preparation of potassium fluoride adopts a neutralization method of taking hydrofluoric acid and potassium hydroxide as raw materials. However, based on the requirement of reducing the production cost, a plurality of domestic enterprises begin to prepare potassium fluoride products by taking industrial byproduct potassium fluosilicate as a raw material.
White carbon black is a general term for white powdery X-ray amorphous silicic acid and silicate products, mainly referring to precipitated silica, fumed silica and ultrafine silica gel, and also including powdery synthetic aluminum silicate, calcium silicate, and the like. The white carbon black is porous material, and its composition can be SiO2·nH2O represents, wherein nH2O is present in the form of surface hydroxyl groups. It is soluble in caustic alkali and hydrofluoric acid, and insoluble in water, solvent and acid (except hydrofluoric acid). High-temperature resistance, non-combustion, tastelessness, odorless and good electrical insulation.
The white carbon black is largely classified into precipitated white carbon black and fumed white carbon black according to the production method. The fumed silica is white amorphous flocculent semitransparent solid colloidal nano particles (the particle size is less than 100nm) in a normal state, is nontoxic and has a huge specific surface area. The fumed silica is completely nano silicon dioxide, the product purity can reach 99%, the particle size can reach 10-20 nm, but the preparation process is complex and the price is high; the precipitated silica is classified into conventional precipitated silica and special precipitated silica, the former is prepared from sulfuric acid, hydrochloric acid, and CO2The silicon dioxide produced by taking water glass as a basic raw material refers to the silicon dioxide produced by adopting a special method such as a supergravity technology, a sol-gel method, a chemical crystal method, a secondary crystallization method or a reversed-phase micelle microemulsion method. The precipitated white carbon black is mainly used as a reinforcing agent of natural rubber and synthetic rubber, a toothpaste friction agent and the like. The fumed silica is mainly used as a reinforcing agent, a coating and an unsaturated resin thickener of the silicone rubber, and the ultrafine silica gel and the aerogel are mainly used as a coating flatting agent, a thickener, a plasticizer, a,Plastic film opening agents, and the like.
The potassium fluoride is prepared by reacting potassium fluosilicate serving as a raw material with a potassium hydroxide solution, so that the cost of the potassium fluoride is obviously reduced; and the quality of the potassium fluoride product can completely reach the level of a neutralization method using hydrofluoric acid through process control. But the method has the disadvantages that silicon elements brought by the potassium fluosilicate raw material are difficult to recover by a precipitation method, and the silicon elements can only be used as an initial silicon source after being washed and recovered in a silicon slag form, so that the value is greatly reduced. But also can pollute the environment when being discarded as waste. In fact, the method is a common problem faced by the enterprises using potassium fluosilicate as a raw material to prepare potassium fluoride at present, and is also a hot spot of research of researchers in the industry. Particularly, at present, the environmental management is increasingly strengthened, and how to change the silicon dioxide byproduct of the process into qualified precipitated white carbon black is particularly important.
The main reason that qualified precipitated silica is difficult to obtain by the prior art is that a potassium hydroxide solution belongs to strong alkali, and silica gel seed crystals are difficult to generate in the initial stage of alkaline hydrolysis, so that the formation of silica particles in the process of aggregation and precipitation during the alkaline hydrolysis process cannot be effectively controlled to obtain the qualified precipitated silica.
In fact, the use of fluorosilicates for fluorine salt production has been a trend in recent years. Traditionally, industrial ammonia water is generally used for decomposing fluosilicic acid or fluosilicate, and self-produced seed crystals are introduced through step-by-step reaction, so that the silicon dioxide which is a byproduct in the ammonolysis process can be directly recovered as white carbon black by a precipitation method, and a batch of patent achievements are formed. For example, CN101428806A (application No. CN200810239646) discloses a large-scale production method for preparing high-reinforcement white carbon black by using fluosilicic acid as a raw material, which is characterized in that: when fluosilicic acid is used as a raw material, liquid ammonia, gas ammonia or ammonia water is used for neutralizing the fluosilicic acid into an ammonium fluosilicate solution in advance, and the ammonium fluosilicate solution is aminolyzed by two steps of ammonia addition. Wherein, in the first step, the seed crystal is obtained by quickly adding ammonia, and then the high-reinforcement white carbon black is obtained by controlling the technological parameters in the second step. The patent becomes a method commonly used in research or production of fluosilicic acid or fluosilicic acid salt by adopting an ammonolysis method to prepare the fluosilicate in recent years in China.
The research on the alkaline hydrolysis reaction process of potassium fluosilicate and potassium hydroxide solution shows that the reaction process cannot form silicon gel crystal seeds like a rapid ammonia adding method in a similar ammonolysis method, and then the formation and aggregation precipitation of silicon dioxide particles in the reaction process are controlled by the crystal seeds. This is because potassium hydroxide, sodium hydroxide and the like are strongly alkaline, and after the alkaline hydrolysis agent is rapidly added, the silicon dioxide nuclei formed by alkaline hydrolysis are dissolved away and also cover the surface of the unreacted fluosilicate to hinder the alkaline hydrolysis reaction when the fluosilicate is rapidly alkaline-hydrolyzed. The equilibrium is broken only at higher temperatures and the alkaline hydrolysis reaction is allowed to complete instantaneously. A large number of colloidal silica particles are formed which are not easily washed by filtration and which are inactive. The potassium fluosilicate and the potassium hydroxide solution react in the alkaline hydrolysis process as follows:
K2SiF6+4KOH→6KF+SiO2↓+2H2O (1)
side reactions also occur
MSiO2+nKOH→MSiO2.nSiO2+H2O (2)
The complex alkaline hydrolysis process increases the difficulty of controlling the degradation reaction (1), so that the silicon dioxide particles precipitated by the reaction (1) can not be orderly aggregated and grown. Therefore, the difficulty of obtaining high-quality white carbon black by using potassium hydroxide to reduce potassium fluosilicate is very large.
CN103112873B (application No. 201310059606.8) adopts ammonolysis mode to process potassium fluosilicate to obtain mixed solution of ammonium fluoride and potassium fluoride, after separating out by-product silicon dioxide product, uses potassium hydroxide solution and mixed solution to carry out deamination reaction, finally obtains potassium fluoride product. CN103101931A (application number CN201310060817) also relates to a method for preparing potassium fluoride and co-producing white carbon black by using potassium fluosilicate, wherein potassium fluosilicate slurry and potassium carbonate solution react to obtain mixed slurry, the potassium fluosilicate slurry with the mass concentration of 10-40% and the potassium carbonate solution with the mass concentration of 10-50% react at 50-105 ℃ for 0.5-2 hours to obtain mixed slurry containing potassium fluoride solution and silicon dioxide solids, and carbon dioxide gas is discharged; the two patent applications focus on the preparation of potassium fluoride products, and the white carbon black is obtained while the potassium fluoride is prepared. However, a different route of starting materials was used.
Chinese patent document CN103979548A (application No. 201410237428.8) discloses a new process for producing fluoride and co-producing white carbon black by fluosilicic acid or fluosilicate, and the invention promotes SiO by adding exogenous seed crystals into reaction solution2The heterogeneous nucleation can accelerate the hydrolysis rate of the fluosilicate and improve the reaction efficiency; the reaction rate of high-temperature hydrolysis in the conventional method can be achieved at a relatively mild reaction temperature. Added SiO2The amount of crystal grains is SiO generated by reaction21 per mill-10% of the total amount. It is clear that the focus of the process is not to increase the quality of the silica by-product, but to lower the temperature of the alkaline hydrolysis.
Disclosure of Invention
Based on the above, the invention aims to provide a process for co-producing white carbon black by adding silica gel seed crystals when potassium fluosilicate is used for producing potassium fluoride. The invention uses fluosilicic acid to synthesize silica gel seed crystal, uses the silica gel seed crystal as an additional seed crystal, and carries out alkaline hydrolysis on potassium fluosilicate to prepare potassium fluoride and coproduce white carbon black.
In order to achieve the purpose, the invention provides the following scheme:
a process for co-producing white carbon black by adding silica gel crystal seeds when potassium fluoride is produced by utilizing potassium fluosilicate comprises the following steps:
(1) reacting industrial by-product fluosilicic acid serving as a raw material with potassium hydroxide at a certain temperature to form a silica gel seed crystal in the stirring process, stopping stirring, and then performing aging treatment to prepare silica plus silica gel seed crystal;
(2) stirring and smashing the silica gel seed crystal after aging treatment to be used as a base material, heating to 80-95 ℃, simultaneously adding a potassium hydroxide solution and potassium fluosilicate, carrying out alkaline hydrolysis reaction to obtain a potassium fluoride solution and precipitate silica, wherein the precipitated silica particles are aggregated under the action of the silica gel seed crystal to form precipitated white carbon black, and weighing the potassium hydroxide and the potassium fluosilicate according to the stoichiometric ratio of the following chemical reaction equation:
K2SiF6+4KOH→6KF+SiO2↓+2H2O (1)；
(3) and filtering and washing the mixture of the precipitated white carbon black and potassium fluoride to obtain a precipitated silicon dioxide filter cake, drying to obtain a white carbon black product, and concentrating and drying the filtrate to obtain a potassium fluoride product.
Preferably, the silica gel seed crystal is prepared by taking an industrial byproduct fluorosilicic acid solution as a raw material and reacting the industrial byproduct fluorosilicic acid solution with a potassium hydroxide solution.
Further preferably, the concentration of the industrial byproduct fluorosilicic acid solution is 20-40%; the concentration of the potassium hydroxide solution is 20-48%; the ratio of fluosilicic acid to potassium fluosilicate in the subsequent alkaline hydrolysis reaction is 1: 1.5 to 3.0.
Specifically, the silicon gel seed crystal preparation process has the following control parameters: heating the fluosilicic acid solution to 40-70 ℃ under stirring, then adding the potassium hydroxide solution into the fluosilicic acid solution at a certain speed until silicon gel is formed, stopping stirring, and standing and aging to obtain additional gel seed crystals.
Preferably, the aging time in the step (2) is 30-60 min.
Preferably, the reaction time of the potassium fluosilicate and the potassium hydroxide in the alkaline hydrolysis reaction process in the step (3) is 60-120 min, and the pH is controlled to be 7-10 in the alkaline hydrolysis process.
The reaction mechanism of the silica gel seed crystal of the present invention is as follows:
H2SiF6+2KOH→K2SiF6+2H2O (3)
K2SiF6+4KOH→6KF+SiO2↓+2H2O (1)
according to the reaction, a certain amount of potassium hydroxide solution is quickly added into a certain amount of fluorosilicic acid solution under stirring, firstly potassium fluosilicate fine particles are quickly formed according to the reaction (3), and the potassium hydroxide solution continuously and quickly reacts according to the reaction (1) before potassium fluosilicate precipitates are formed by growth. Under the condition of a certain temperature, the colloidal silicon dioxide solution forms silica gel crystal seeds under the action of a colloidal electrolyte potassium fluoride solution.
Compared with the prior art, the invention discloses the following technical effects: the fluorosilicic acid solution adopted by the invention is anhydrous hydrogen fluoride or a phosphate fertilizer industrial byproduct, and the ideal silica gel can be prepared by taking the fluorosilicic acid solution as a raw material without introducing other impurities. By controlling the amount of the introduced silica gel crystal seeds and the technological parameters of the alkaline hydrolysis process, the qualified potassium fluoride product can be prepared by using potassium fluosilicate as a raw material to react with a potassium hydroxide solution, and meanwhile, a precipitated silica white byproduct with adjustable indexes meeting the national standard requirement can be obtained.
The invention makes the process for preparing the potassium fluoride by using the potassium fluosilicate and the potassium hydroxide as basic raw materials more complete and has good popularization prospect.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a process for co-producing white carbon black by adding silica gel crystal seeds when potassium fluosilicate is used for producing potassium fluoride.
The present invention will be described in further detail with reference to specific embodiments in order to make the above objects, features and advantages more apparent and understandable.
Example 1
(1) 1100g of 40% industrial fluosilicic acid is taken and added with water to prepare 20 wt% fluosilicic acid solution, the temperature is raised to 45 ℃ under stirring, then 3170g of 20% potassium hydroxide solution is rapidly added within 5min, the mixed reaction solution forms silicon gel under stirring, the stirring is stopped, and the mixture is kept still and aged for 30 min;
(2) stirring, scattering silica gel seed crystals, heating to 85 ℃, slowly adding 1300g of potassium fluosilicate and 4830g of 48% potassium hydroxide solution, controlling the adding time to be 60-90min, and controlling the pH value of reaction slurry to be 8.0-8.5; after the reaction is finished, continuously stirring the reaction slurry for 30min, and then stopping stirring to obtain mixed slurry;
(3) the resulting mixed slurry was filtered to obtain a filter cake of solid silica and 10420g of a filtrate containing 23.30% by weight of a potassium fluoride solution;
(4) the precipitated silica filter cake obtained by filtration is subjected to a washing operation to recover potassium fluoride entrained in the filter cake and washed to neutrality. The filter cake is easy to wash, and 570g of white carbon black product is prepared after the filter cake is dried for 3 hours at 120 ℃. The obtained white carbon black product has the main technical indexes that: specific surface area 145m2(ii)/g; DBP oil absorption number 2.78; the ignition loss is 6.7%.
Example 2
(1) 1130g of 40 percent industrial fluosilicic acid is taken and added with water to prepare 20 percent fluosilicic acid solution by weight, the temperature is raised to 45 ℃ under stirring, then 3690g of corresponding 20 percent potassium hydroxide solution by weight is rapidly added within 5min, the mixed reaction solution forms silica gel under stirring, the stirring is stopped, and the mixture is kept still and aged for 30 min;
(2) starting stirring, breaking and dispersing the silica gel seed crystal, simultaneously heating to 85 ℃, slowly adding 1200g of potassium fluosilicate and 4100g of 48% potassium hydroxide solution corresponding to the potassium fluosilicate under stirring, controlling the adding time to be 60-90min, and keeping the pH value in the reaction process to be 8.5-9.0. After the reaction is finished, continuously stirring and reacting for 30min, and then stopping stirring to obtain mixed slurry;
(3) the resulting mixed slurry was filtered to obtain a filter cake of solid silica and 10390g of a filtrate containing 22.64% by weight of a potassium fluoride solution; the material is easy to filter, and filtrate is refined, concentrated and spray-dried to obtain 2235g of superior potassium fluoride.
(4) Filtering to obtain precipitated silica filter cake, washing to recover potassium fluoride carried in the filter cake, and washing to neutrality. The filter cake is easy to wash, the filter cake is dried for 3 hours at 120 ℃ to prepare 540g of white carbon black product, and the obtained white carbon black product has the main technical indexes that: specific surface area 195m2(ii)/g; DBP oil absorption number 2.98; the ignition loss is 7.2%.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the system disclosed by the embodiment, the description is relatively simple because the system corresponds to the method disclosed by the embodiment, and the relevant points can be referred to the method part for description.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (6)
1. A process for co-producing white carbon black by adding silica gel crystal seeds when potassium fluoride is produced by utilizing potassium fluosilicate is characterized by comprising the following steps:
(1) reacting industrial byproduct fluorosilicic acid solution serving as a raw material with potassium hydroxide at a certain temperature to form silica gel seed crystals in the stirring process, stopping stirring, and performing aging treatment to obtain the silica gel seed crystals;
(2) stirring and smashing the prepared additional silica gel seed crystal serving as a base material, heating to 80-95 ℃, simultaneously adding a potassium hydroxide solution and potassium fluosilicate, carrying out alkaline hydrolysis reaction to obtain a potassium fluoride solution and precipitate silica particles, wherein the precipitated silica particles are aggregated under the action of the silica gel seed crystal to form precipitated silica. Weighing potassium hydroxide and potassium fluosilicate according to the stoichiometric ratio of the following chemical reaction equation:
K2SiF6+4KOH→6KF+SiO2↓+2H2O(1)；
(3) and filtering and washing the mixture of the precipitated white carbon black and potassium fluoride to obtain a precipitated silicon dioxide filter cake, drying to obtain a white carbon black product, and concentrating and drying the filtrate to obtain a potassium fluoride product.
2. The process for co-producing white carbon black by adding silica gel seed crystals during the production of potassium fluoride by using potassium fluosilicate according to claim 1, wherein the silica gel seed crystals in the step (1) are prepared by reacting industrial by-product fluorosilicic acid solution serving as a raw material with potassium hydroxide solution.
3. The process for co-producing white carbon black by adding silica gel seed crystals during the production of potassium fluoride by using potassium fluosilicate according to claim 2, wherein the concentration of the industrial byproduct fluosilicate solution is 20-40%; the concentration of the potassium hydroxide solution is 20-48%; the ratio of fluosilicic acid to potassium fluosilicate in the subsequent alkaline hydrolysis reaction is 1: 1.5 to 3.0.
4. The process for co-producing white carbon black by adding silica gel seed crystals during the production of potassium fluoride by using potassium fluosilicate according to claim 3, wherein the control parameters of the silica gel seed crystal preparation process are as follows: heating the fluosilicic acid solution to 40-70 ℃ under stirring, then adding the potassium hydroxide solution into the fluosilicic acid solution at a certain speed until silicon gel is formed, stopping stirring, and standing and aging to obtain the additional silicon gel seed crystal.
5. The process for co-producing white carbon black by adding silica gel seed crystals during the production of potassium fluoride by using potassium fluosilicate according to claim 1, wherein the aging time in the step (1) is 30-60 min.
6. The process for co-producing white carbon black by adding silica gel seed crystals during the production of potassium fluoride by using potassium fluosilicate according to claim 1, wherein the reaction time of potassium fluosilicate and potassium hydroxide is 60-120 min in the alkaline hydrolysis reaction process in the step (2), and the pH value is controlled to be 7-10 in the alkaline hydrolysis process.
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| CN117446833A (en) * | 2023-09-20 | 2024-01-26 | 山东立中新能源材料有限公司 | Preparation method of sodium hexafluorophosphate for sodium battery |
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