CN109480097B - Preparation method of silica microspheres for acidifier carrier - Google Patents
Preparation method of silica microspheres for acidifier carrier Download PDFInfo
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Abstract
The invention discloses a preparation method of silica microspheres for an acidifier carrier, which comprises the following steps: adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring for heating, adding water for stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, firstly acidifying to a certain pH value, and simultaneously adding sulfuric acid and sodium silicate into the obtained reaction liquid B for synthesis reaction to obtain a reaction liquid C; then stopping adding the sodium silicate, only adding sulfuric acid, acidifying to a certain pH value, and curing to obtain a dilute slurry D; and filtering, washing, pulping, thickening and drying the thin slurry D to obtain the silica microspheres for the acidifier carrier. The silicon dioxide microspheres provided by the invention have uniform particle size, are not easy to break, are not agglomerated, and have high adsorption speed, good free-running property and good adsorbability.
Description
Technical Field
The invention relates to the field of preparation of silicon dioxide, and particularly relates to a preparation method of silicon dioxide microspheres for an acidifier carrier.
Background
The feed additive acidifier is an important additive which is juxtaposed with probiotics, enzyme preparations, microecologics and the like after antibiotics, and is an environment-friendly additive without residues, drug resistance and toxic action. In recent years, acidifying agent, probiotics, enzyme preparation, flavoring agent and the like are combined into a novel green feed additive, and the application of the feed acidifying agent in the fields of piglet feed, poultry feed, silage and the like is increasingly common and has obvious effect. However, some problems exist, such as unstable use effect of the acidifier, high cost, difficult dispersion of the prepared premix, too fast absorption in animal stomach, easy moisture absorption and agglomeration, and corrosion to processing machinery, transportation equipment, etc. The quality of the acidulant product is influenced by the content of the active ingredients, and has a very close relationship with the performance of the carrier. The carrier is generally silicon dioxide, at present, the preparation method of the silicon dioxide mainly comprises a precipitation method and a gas phase method, and the precipitation method is dominant because the raw materials used are cheap and easy to obtain, the production process and equipment are simpler, and the product is low in price. The precipitation method mainly comprises the steps of preparing dilute solution with a certain concentration by adopting industrial water glass, then adding certain acid under a certain condition to precipitate silicon dioxide, and then cleaning, filtering, drying and crushing to obtain the silicon dioxide. However, most of the silica carriers used in the prior acidulant industry are fine powders, which have poor adsorptivity and flowability, are easy to agglomerate, are not easy to disperse, have small addition amount, cannot well meet the use requirements, and even bring about quality accidents, so a preparation method of silica is needed, which has good adsorptivity and flowability, and is stable and not easy to agglomerate.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a preparation method of silica microspheres for an acidifier carrier, which comprises the following steps:
(1): adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring, heating to 75-95 ℃, adding water, stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, and acidifying until the pH value of the solution is 7.5-11.5 to obtain a reaction solution B;
(2): simultaneously adding sulfuric acid and sodium silicate into the reaction liquid B obtained in the step (1) for synthetic reaction to obtain reaction liquid C;
(3): stopping adding sodium silicate into the reaction liquid C obtained in the step (2), only adding sulfuric acid for acidification, detecting that the pH value reaches 3.5-5.5, and curing to obtain a dilute slurry D;
(4): filtering and washing the thin slurry D obtained in the step (3) to obtain a filter cake E, transferring the obtained filter cake E to a pulping machine, and adding a thickening agent to obtain slurry G;
(5): and (4) drying the slurry obtained in the step (4) to obtain the silica microspheres for the acidifier carrier.
In the steps (1) to (3): the sodium silicate is a sodium silicate aqueous solution with the concentration of 20-30 Baume degrees; the modulus of the sodium silicate is 2.80-3.30; the sulfuric acid is a sulfuric acid aqueous solution with the mass fraction of 30-60%.
In the step (1): the addition amount of the sodium silicate is 15-25m3(ii) a The concentration of sodium silicate in the reaction bottom material A is 13-15 Baume degrees; the flow velocity of the sulfuric acid is 5-10m3The adding time of the sulfuric acid is 40-60min, and the stirring speed is 22-57 rpm.
In the step (2): the flow velocity of the sulfuric acid is 5-10m3H, the flow rate of the sodium silicate is 15m3And h, the charging time of the sulfuric acid and the sodium silicate is 15-30 min.
In the step (3): the flow rate of the sulfuric acid is 50-70% of that of the sulfuric acid in the step (2), and the feeding time of the sulfuric acid is 30-40 min; the curing time is 5-15 min.
The thickener in the step (4) is a polycarboxylic acid thickener; preferably, the polycarboxylic acid thickener is sodium polyacrylate.
In the step (4): the conductivity of the drained water in the washing process is 5.0-10.0 ms/cm.
In the step (5): the drying method comprises the steps of carrying out first-stage drying after pressure spray drying, and then entering a fluidized bed for second-stage drying; the temperature of the first-stage drying is 350-550 ℃, and the pressure of the first-stage drying is-50 to-250 Pa; the temperature of the second-stage drying is 150-250 ℃, and the second-stage drying pressure is-350 to-150 Pa;
the invention has the beneficial effects that:
(1) the invention provides a production technology of silica microspheres, which has the advantages of coarsened product appearance, certain strength, uniform particle size of the microspheres, no crushing and agglomeration in the process of adsorbing an acidifying agent, high adsorption speed, good free-running property and adsorbability, capability of improving the quality level and production efficiency of the acidifying agent and reduction of the manufacturing cost of a feed acidifying agent.
(2) According to the invention, the silicon dioxide microspheres for the acidifier carrier prepared by adjusting the modulus of sodium silicate in sodium silicate, the concentration of sodium silicate and sulfuric acid in each step and the adding time have high adsorbability.
(3) According to the invention, the polycarboxylic acid thickener is selected, so that the viscosity of the material before drying is increased, and the surface hardness of the dried product and the particle strength of the silicon dioxide microspheres are improved.
(4) According to the invention, the drying mode of combining pressure spray drying with a fluidized bed is adopted, and the fluidized bed is dried by using clean air heated indirectly by steam, so that the granularity, strength and free-running property of the product are ensured, the forming of the acidifying agent is facilitated, and the stability of the acidifying agent is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
EXAMPLE 1 preparation of silica microspheres for acidifier Carrier
The method comprises the following steps:
(1): adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring, heating to 75 ℃, adding water, stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, and acidifying until the pH value of the solution is 8.0 to obtain a reaction solution B;
(2): simultaneously adding sulfuric acid and sodium silicate into the reaction liquid B obtained in the step (1) for synthetic reaction to obtain reaction liquid C;
(3): stopping adding sodium silicate into the reaction liquid C obtained in the step (2), only adding sulfuric acid for acidification, detecting that the pH value reaches 4.5, and curing to obtain a dilute slurry D;
(4): filtering and washing the thin slurry D obtained in the step (3) to obtain a filter cake E, transferring the obtained filter cake E to a pulping machine, and adding a thickening agent to obtain slurry G;
(5): and (4) drying the slurry obtained in the step (4) to obtain the silica microspheres for the acidifier carrier.
In the steps (1) to (3): the sodium silicate is a sodium silicate aqueous solution with the concentration of 20 Baume degrees; the modulus of the sodium silicate is 2.80; the sulfuric acid is a 60% sulfuric acid aqueous solution.
In the step (1): the addition amount of the sodium silicate is 15m3(ii) a The concentration of sodium silicate in the reaction bottom material A is 14.3 Baume degrees; the flow velocity of the sulfuric acid is 5m3The addition time of the sulfuric acid is 45min, and the stirring speed is 35 rpm.
In the step (2): the flow velocity of the sulfuric acid is 5m3H, the flow rate of the sodium silicate is 15m3The charging time of the sulfuric acid and the sodium silicate is 20 min.
In the step (3): the flow rate of the sulfuric acid is 2.5m in the step (2)3The charging time of the sulfuric acid is 30 min; the curing time is 10 min.
The thickener in the step (4) is sodium polyacrylate, the addition amount of the sodium polyacrylate is 5.0kg, and the pH value of the slurry G is 6.3.
In the step (4): the conductivity of the drain water during the washing process was 5.0 ms/cm.
In the step (5): the drying method comprises the steps of carrying out first-stage drying after pressure spray drying, and then entering a fluidized bed for second-stage drying; the temperature of the first-stage drying is 450 ℃, and the first-stage drying pressure is-50 Pa; the temperature of the second-stage drying is 160 ℃, and the pressure of the second-stage drying is-200 Pa.
Example 2A method for preparing silica microspheres for acidifying agent carrier
The method comprises the following steps:
(1): adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring, heating to 95 ℃, adding water, stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, and acidifying until the pH value of the solution is 10.0 to obtain a reaction solution B;
(2): simultaneously adding sulfuric acid and sodium silicate into the reaction liquid B obtained in the step (1) for synthetic reaction to obtain reaction liquid C;
(3): stopping adding sodium silicate into the reaction liquid C obtained in the step (2), only adding sulfuric acid for acidification, detecting that the pH value reaches 4.5, and curing to obtain a dilute slurry D;
(4): filtering and washing the thin slurry D obtained in the step (3) to obtain a filter cake E, transferring the obtained filter cake E to a pulping machine, and adding a thickening agent to obtain slurry G;
(5): and (4) drying the slurry obtained in the step (4) to obtain the silica microspheres for the acidifier carrier.
In the steps (1) to (3): the sodium silicate is a sodium silicate aqueous solution with the concentration of 30 Baume degrees; the modulus of the sodium silicate is 3.30; the sulfuric acid is a 30% sulfuric acid aqueous solution by mass fraction.
In the step (1): the adding amount of the sodium silicate is 25m3(ii) a The concentration of sodium silicate in the reaction bottom material A is 10.5 Baume degrees; the flow velocity of the sulfuric acid is 10m3The addition time of the sulfuric acid is 60min, and the stirring speed is 22 rpm.
In the step (2): the flow velocity of the sulfuric acid is 10m3H, the flow rate of the sodium silicate is 15m3The charging time of the sulfuric acid and the sodium silicate is 30 min.
In the step (3): the flow velocity of the sulfuric acid is 5m3The charging time of the sulfuric acid is 30 min; the curing time is 15 min.
The thickening agent in the step (4) is sodium polyacrylate, the addition amount of the sodium polyacrylate is 10.0kg, and the pH value of the slurry G is 6.9.
In the step (4): the conductivity of the drain water in the washing process was 8.0 ms/cm.
The drying process in the step (5) is that after pressure spray drying, first-stage drying is carried out, and then the drying is carried out in a fluidized bed for second-stage drying, wherein the fluidized bed drying selects clean air indirectly heated by steam; the temperature of the first-stage drying is 550 ℃, and the first-stage drying pressure is-150 Pa; the temperature of the second-stage drying is 210 ℃, and the pressure of the second-stage drying is-200 Pa.
Example 3A method for preparing silica microspheres for acidifier carrier
The method comprises the following steps:
(1): adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring, heating to 85 ℃, adding water, stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, and acidifying until the pH value of the solution is 9.5 to obtain a reaction solution B;
(2): simultaneously adding sulfuric acid and sodium silicate into the reaction liquid B obtained in the step (1) for synthetic reaction to obtain reaction liquid C;
(3): stopping adding sodium silicate into the reaction liquid C obtained in the step (2), only adding sulfuric acid for acidification, detecting that the pH value reaches 4.5, and curing to obtain a thin slurry material D;
(4): filtering and washing the thin slurry D obtained in the step (3) to obtain a filter cake E, transferring the obtained filter cake E to a pulping machine, and adding a thickening agent to obtain slurry G;
(5): and (4) drying the slurry obtained in the step (4) to obtain the silica microspheres for the acidifier carrier.
In the steps (1) to (3): the sodium silicate is a sodium silicate aqueous solution with the concentration of 20 Baume degrees; the modulus of the sodium silicate is 3.30; the sulfuric acid is a 60% sulfuric acid aqueous solution.
In the step (1): the adding amount of the sodium silicate is 25m3(ii) a The concentration of sodium silicate in the reaction bottom material A is 12 Baume degrees; the flow velocity of the sulfuric acid is 6.0m3The addition time of the sulfuric acid is 50min, and the stirring speed is 22 rpm.
In the step (2): the flow velocity of the sulfuric acid is 8m3H, the flow rate of the sodium silicate is 15.0m3The charging time of the sulfuric acid and the sodium silicate is 20 min.
In the step (3): the flow velocity of the sulfuric acid is 5.0m3The charging time of the sulfuric acid is 30 min; the curing time is 15 min.
The thickening agent in the step (4) is sodium polyacrylate, the adding amount of the sodium polyacrylate is 10.0Kg, and the pH value of the slurry G is 6.6.
In the step (4): the conductivity of the drain water in the washing process was 8.0 ms/cm.
The drying process in the step (5) is that after pressure spray drying, first-stage drying is carried out, and then the drying is carried out in a fluidized bed for second-stage drying, wherein the fluidized bed drying selects clean air indirectly heated by steam; the temperature of the first-stage drying is 550 ℃, and the first-stage drying pressure is-150 Pa; the temperature of the second-stage drying is 210 ℃, and the pressure of the second-stage drying is-200 Pa.
Comparative example 1 preparation method of silica microspheres for acidifier carrier
The preparation method is basically the same as that of the example 1, and the difference from the example 1 is that: the modulus of the sodium silicate is 3.55.
Comparative example 2 preparation method of silica microspheres for acidifier carrier
The preparation method is basically the same as that of the example 1, and the difference from the example 1 is that: the thickening agent is sodium bicarbonate.
The acidulant carrier prepared by the preparation methods of examples 1-3 and comparative examples 1-2 above was subjected to performance tests using silica microspheres, the test results are shown in the following table:
TABLE 1
As can be seen from the data in Table 1, the acidulant carrier silicas provided in examples 1-3 of the invention have DBP absorption of the microspheres in the range of 2.55 to 2.80ml/g, which is higher than that of comparative example 1.
TABLE 2
As can be seen from the data in Table 2, the silica microspheres for acidifier carriers provided in examples 1 to 3 of the present invention have good thermal stability, high hardness, low particle breakage and effective adsorption of fumaric acid.
TABLE 3
As can be seen from the data in Table 3, the silica microspheres as acidifier carriers provided in examples 1 to 3 of the present invention have a high specific surface area, and are excellent in dispersibility and free from agglomeration.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Claims (6)
1. A preparation method of silica microspheres for an acidifier carrier is characterized by comprising the following steps: (1): adding sodium silicate into a synthesis kettle, introducing steam under the condition of stirring, heating to 75-95 ℃, adding water, stirring to obtain a reaction bottom material A, adding sulfuric acid into the reaction bottom material A, and acidifying until the pH value of the solution is 7.5-11.5 to obtain a reaction solution B; (2): simultaneously adding sulfuric acid and sodium silicate into the reaction liquid B obtained in the step (1) for synthetic reaction to obtain reaction liquid C; (3): stopping adding sodium silicate into the reaction liquid C obtained in the step (2), only adding sulfuric acid for acidification, detecting that the pH value reaches 3.5-5.5, and curing to obtain a dilute slurry D; (4): filtering and washing the thin slurry D obtained in the step (3) to obtain a filter cake E, transferring the obtained filter cake E to a pulping machine, and adding a thickening agent to obtain slurry G; (5): drying the slurry obtained in the step (4) to obtain the silica microspheres for the acidifier carrier; in the steps (1) to (3): the sodium silicate is a sodium silicate aqueous solution with the concentration of 20-30 Baume degrees; the modulus of the sodium silicate is 2.80-3.30; the sulfuric acid is a sulfuric acid aqueous solution with the mass fraction of 30-60%; the thickener in the step (4) is a polycarboxylic acid thickener; in the step (5): the drying method is that the first stage drying is carried out by a pressure spray drying mode, and then the drying enters an ebullated bed for the second stage drying.
2. The process for producing silica microspheres for acidifying agent carrier according to claim 1, whereinIn the step (1): the addition amount of the sodium silicate is 15-25m3(ii) a The concentration of sodium silicate in the reaction bottom material A is 13-15 Baume degrees; the flow rate of the sulfuric acid is 5-10m3/h, the adding time of the sulfuric acid is 40-60min, and the stirring speed is 22-57 rpm.
3. The process for producing silica microspheres for an acidulant carrier as claimed in claim 1, wherein in step (2): the flow velocity of the sulfuric acid is 5-10m3H, the flow rate of the sodium silicate is 15m3And h, the charging time of the sulfuric acid and the sodium silicate is 15-30 min.
4. The process for preparing silica microspheres for acidulant carrier as claimed in claim 1, wherein in step (3): the flow rate of the sulfuric acid is 50-70% of that of the sulfuric acid in the step (2), and the feeding time of the sulfuric acid is 30-40 min; the curing time is 5-15 min.
5. The process for preparing silica microspheres for acidulant carrier as claimed in claim 1, wherein in step (4): the conductivity of the drained water in the washing process is 5.0-10.0 ms/cm.
6. The method for preparing silica microspheres for an acidifier carrier according to claim 1, wherein the temperature of the first stage drying is 350-550 ℃, and the pressure of the first stage drying is-250 to-50 Pa; the temperature of the second-stage drying is 150-250 ℃, and the pressure of the second-stage drying is-350 to-150 Pa.
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| PCT/CN2019/085748 WO2020140358A1 (en) | 2019-01-03 | 2019-05-07 | Method for preparing silica microspheres for acidifier carrier |
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| CN112520747A (en) * | 2020-12-16 | 2021-03-19 | 冷水江三A新材料科技有限公司 | Micron-sized iron-doped silicon dioxide and preparation method and application thereof |
| CN112694092A (en) * | 2020-12-29 | 2021-04-23 | 山东联科卡尔迪克白炭黑有限公司 | Production process and application of silicon dioxide for choline chloride carrier |
| CN114735713B (en) * | 2022-03-02 | 2024-03-29 | 福建同晟新材料科技股份公司 | Preparation process of synthetic silicon dioxide for papermaking additive |
| CN115710000A (en) * | 2022-09-08 | 2023-02-24 | 确成硅化学股份有限公司 | Preparation method of special white carbon black for storage battery separator |
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| CN103435048A (en) * | 2013-08-17 | 2013-12-11 | 福建省三明同晟化工有限公司 | Preparation method of silicon dioxide used for tooth paste |
| CN107720763A (en) * | 2017-11-21 | 2018-02-23 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high dispersive silica |
| CN108821298A (en) * | 2018-08-16 | 2018-11-16 | 广州市飞雪材料科技有限公司 | A kind of high absorption high dispersive silica and preparation method thereof |
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| FR2767071B1 (en) * | 1997-08-06 | 1999-09-10 | Rhodia Chimie Sa | COMPOSITION COMPRISING A LIQUID ABSORBED ON A PRECIPITATED SILICA BASE |
| FR2843894B1 (en) * | 2002-08-30 | 2004-11-12 | Rhodia Chimie Sa | COMPOUND FORMING PRECIPITATED SILICA AND PHOSPHATE AND ITS USE AS A NUTRITIONAL LIQUID SUPPORT AND AS A NUTRITIONAL ANTIMOTANT AGENT |
| JP5868520B2 (en) * | 2011-12-23 | 2016-02-24 | ローディア オペレーションズ | Method for producing precipitated silica |
| CN104276577B (en) * | 2014-09-22 | 2016-08-24 | 无锡恒诚硅业有限公司 | A kind of have the precipitated silica of granule homogeneity, preparation method and its usage |
| CN104760961A (en) * | 2014-12-16 | 2015-07-08 | 安徽确成硅化学有限公司 | Production method for functional silica |
| CN105060307B (en) * | 2015-09-09 | 2017-04-05 | 确成硅化学股份有限公司 | A kind of high-specific surface area white carbon and its production method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435048A (en) * | 2013-08-17 | 2013-12-11 | 福建省三明同晟化工有限公司 | Preparation method of silicon dioxide used for tooth paste |
| CN107720763A (en) * | 2017-11-21 | 2018-02-23 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high dispersive silica |
| CN108821298A (en) * | 2018-08-16 | 2018-11-16 | 广州市飞雪材料科技有限公司 | A kind of high absorption high dispersive silica and preparation method thereof |
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