CN112694092A - Production process and application of silicon dioxide for choline chloride carrier - Google Patents
Production process and application of silicon dioxide for choline chloride carrier Download PDFInfo
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Abstract
The invention discloses a production process of silicon dioxide for a choline chloride carrier, which comprises seed crystal preparation, first-stage synthesis, second-stage synthesis, semi-finished product preparation and final product preparation, wherein the final product is a final product which is prepared by sieving to remove fine powder with the mesh number larger than 200 after the final product preparation is finished and then packaging in a vacuum negative pressure state. In addition, the invention also discloses application of the silicon dioxide prepared by the preparation process as a choline chloride carrier. The silica product prepared by the process has good fluidity, does not raise dust or agglomerate in the choline chloride adsorption process, has excellent adsorption performance, and has obvious advantages of adsorbability and manufacturing cost compared with the existing granular carrier.
Description
Technical Field
The invention relates to the technical field of silicon dioxide preparation, in particular to a production process and application of silicon dioxide for a choline chloride carrier.
Background
Choline is an indispensable basic component in the body of animals, and most animals cannot meet the growth and development of choline synthesized by themselves and must be ingested through the outside. The artificially synthesized choline chloride as the feed additive for livestock can stimulate the ovary to produce more eggs and farrowing, promote the absorption and synthesis of amino acid in the bodies of the livestock, enhance the physique and disease resistance of the livestock and promote the growth and development of the livestock and the poultry. The choline chloride is a choline salt, and molecules of the choline chloride have a polar tendency, so the choline chloride is extremely easy to absorb moisture, brings certain difficulty to production, processing, storage and feeding, is extremely easy to agglomerate and mildew, and affects quality. Therefore, the choice of which carrier is suitable is of great importance in the production process in relation to the resistance to moisture agglomeration. Currently, the silicon-type choline chloride is the mainstream in the international market, and the characteristics of physiological inertia and high adsorbability of silicon dioxide are utilized to be used as a carrier of the choline chloride, so that the product performance is excellent, and the demand is considerable. However, the silica supports made in China generally have the following problems: the silica product has low oil absorption value, high water content, high sulfate content and small pore volume, and the adsorption effect of the silica on choline chloride when being used as a carrier is seriously limited; the silicon dioxide product has small specific gravity and wide particle size distribution, so that the silicon dioxide product has poor self-fluidity and is easy to aggregate. The defects greatly limit the share of the domestic silicon dioxide in the international choline chloride carrier market.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a production process and application of silicon dioxide for a choline chloride carrier. The production process of the silica for the choline chloride carrier is designed to be a brand-new product manufacturing process, and finally, the high-adsorbability silica product with extremely low fine powder content and uniform particle size is obtained.
The technical scheme of the invention is as follows:
a process for producing silicon dioxide for choline chloride carrier comprises the following steps,
s1: preparing seed crystals, namely adding sodium silicate stock solution into a synthesis kettle, wherein the modulus of the sodium silicate stock solution is 3.0-3.2, the concentration of the sodium silicate stock solution is 0.8-1.8 mol/L, introducing process steam under the stirring state of the synthesis kettle, heating to 40-60 ℃, adding process water to adjust the concentration of the liquid sodium silicate solution to 0.15-0.45 mol/L, adding sulfuric acid with the concentration of 15-30% into the reaction kettle at the speed of 1250-2500L/h, stopping adding acid when the pH of the reaction solution is 7.0-11.0, and keeping for 15-30 min;
s2: first-stage synthesis, namely raising the temperature to 60-90 ℃, keeping stirring, then adding 30-98% of sulfuric acid at the speed of 60-100L/h, and simultaneously adding the sodium silicate stock solution at the speed of 900-1500L/h, wherein the adding time of the two is 20-50 min;
s3: the second-stage synthesis, namely raising the temperature to 60-90 ℃, keeping stirring, adding 30-98% of sulfuric acid at the speed of 105-150L/h, and simultaneously adding the stock solution of sodium silicate at the speed of 1350-2000L/h, wherein the adding time of the two is 20-40 min;
s4: preparing a semi-finished product, namely adding 30-98% sulfuric acid at the speed of 45-90L/h at the temperature of the step S3 until the pH value of the reaction solution is 3.0-7.0, stopping adding acid, and aging for 30min under a stirring state to obtain a semi-finished product thin slurry;
s5: and (4) preparing a final product, namely filtering the semi-finished product thin slurry obtained in the step S4, washing, liquefying a filter cake, pulping, and drying by using a centrifugal spray drying tower to obtain the final product.
As an alternative of the technical scheme of the invention, the conductivity of the process water is less than or equal to 50 mu s/cm, and the pH value is 7.0-7.5; the pressure of the steam for production is 0.5-1.0 MPa.
As an alternative scheme of the technical scheme of the invention, a box filter is used for filtering in the step S5, the filtering pressure is 0.3-0.8 MPa, the filter cake is transferred to a pulping machine after the filtering is finished and the washing is finished until the conductivity of washing drainage water is 3.0-13.0 ms/cm, and the filter cake is conveyed to the centrifugal spray drying tower for drying by a pressurizing pump when the solid content in the pulp is detected to be 15-25% when the pulp is stirred to be in a flowing state.
As an alternative scheme of the technical scheme of the invention, the sodium silicate stock solution in the step S1 is prepared by adding process water and process steam into a dissolving kettle for dissolving solid sodium silicate, wherein the transparency of the sodium silicate stock solution is less than or equal to 5.0NTU, the soluble solid content of the solid sodium silicate is more than or equal to 99%, the iron content is less than or equal to 0.02%, and the heavy metal content (in terms of pb) is less than or equal to 30 mg/kg.
As an alternative of the technical scheme of the invention, the sulfuric acid in the step S1 to the step S4 is prepared from raw material sulfuric acid, the concentration of the raw material sulfuric acid is 93-98%, the transparency is more than or equal to 80mm, and the heavy metal content (in pb) is less than or equal to 50 mg/kg.
As an alternative of the technical scheme of the invention, the stirring speed in the synthesis kettle is 15-105 rpm.
As an alternative scheme of the technical scheme of the invention, the temperature of hot air inlet of the centrifugal spray drying tower is 200-500 ℃, the temperature of the air outlet is 90-130 ℃, the feeding pressure is 0.1-0.3 MPa, the rotating speed of an atomizer is 5000-11000 rpm, the aperture of an atomizing nozzle is 5-12 mm, and the internal pressure of the centrifugal spray drying tower is-150 Pa-50 Pa.
As an alternative of the technical scheme of the invention, the final product in the step S5 is screened to remove fine powder with the mesh number larger than 200 meshes and then packaged in a vacuum negative pressure state.
As an alternative of the technical scheme of the invention, the pressure of the packing machine is-300 Pa to-100 Pa.
In addition, the invention also discloses application of the silicon dioxide prepared by the preparation process as a choline chloride carrier.
Compared with the prior art, the production process of the silicon dioxide for the choline chloride carrier has the following advantages:
the invention discloses a production process of fine micro-bead-shaped silicon dioxide with low fine powder content, moderate hardness, high porosity and adsorptivity and narrow particle size distribution. The prepared silicon dioxide product has good fluidity, does not raise dust or agglomerate in the choline chloride adsorption process, has excellent adsorption performance, has obvious advantages in adsorption and manufacturing cost compared with the existing granular carrier, has good flowing dispersibility, does not agglomerate or agglomerate in the premixed feed after the choline chloride is adsorbed, greatly improves the addition safety and the storage stability of the choline chloride product, and fundamentally improves the production operation environment.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, 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.
Firstly, solid sodium silicate with the soluble solid content of more than or equal to 99 percent, the iron content of less than or equal to 0.02 percent and the heavy metal content (calculated by pb) of less than or equal to 30mg/kg is added into a dissolving kettle, process water and process steam are added to dissolve the solid sodium silicate into sodium silicate stock solution with the modulus of 3.0-3.2, the concentration of 0.8-1.8 mol/L and the transparency of less than or equal to 5.0NTU, and the sodium silicate stock solution is filtered for later use.
In the case of the example 1, the following examples are given,
a production process of silicon dioxide for choline chloride carrier.
1200L of sodium silicate stock solution with the concentration of 1.6mol/L is added into a synthesis kettle, the stirring speed of the synthesis kettle is kept at 98rpm, steam is introduced, the temperature is raised to 50 ℃, a proper amount of process water is added, the concentration of the sodium silicate solution is adjusted to 0.45mol/L, 25% sulfuric acid is added at the speed of 1250L/h, the acid addition is stopped when the pH value of the reaction solution is 10.0, the time is about 30min, and the stage is the seed crystal preparation process.
Then, after the temperature is increased to 78-83 ℃, 98 percent sulfuric acid and sodium silicate stock solution are added for 40min at the temperature at the flow rates of 60L/h and 900L/h simultaneously, and the synthesis is a one-stage synthesis; and then raising the temperature to 85-90 ℃, and adding 98% sulfuric acid and sodium silicate stock solution at the flow rates of 105L/h and 1350L/h for 30min at the same time, thereby carrying out two-stage synthesis.
Stopping adding the sodium silicate stock solution, reducing the flow rate of 98 percent sulfuric acid to 45L/h at 90 ℃, and stopping adding acid when the pH value of the reaction solution reaches 4.5 after 25 min. And after aging for 30min, pumping the dilute slurry into a filter, washing a filter cake by using process water when a large amount of filtrate does not flow out any more until the drainage conductivity is 5.0ms/cm, stopping washing, transferring the filter cake to a pulping machine, stirring to form a better flowing state, detecting that the solid content of the concentrated slurry is 18.7 percent, and the pH value is 6.5, and pumping to a centrifugal spray drying tower by using a pressurizing pump.
Drying the concentrated slurry in a centrifugal spray drying tower, wherein the temperature of hot air is 350 ℃, the rotating speed of an atomizer is 6200rpm, the outlet temperature is controlled to be 125 +/-5 ℃, the negative pressure is-100 Pa, and the aperture of an atomizing nozzle is 6.0 mm; and (3) packaging the product by using a vacuum packaging machine, controlling the negative pressure of the packaging to be-100 Pa, and controlling the heating decrement of the product to be 4.0-5.0%, thus obtaining a final finished product.
The quality indexes of the silicon dioxide prepared in the production process of the embodiment are tested as follows:
1) (105 ℃/2h) heating loss: 4.3 percent;
2) DOA uptake: 2.7 ml/g;
3) bulk specific gravity: 0.22;
4) pass rate of 40 mesh: 97 percent;
5) the screen-passing rate of 40-80 meshes: 62 percent;
6) 80-120 mesh oversize: 33%;
7) 200 mesh undersize: 2 percent;
8) soluble salt content: 1.85 percent
9) BET specific surface area: 195m2/g；
10) The iron content: 260 ppm;
11) heavy metal content (in pb): 5.9 ppm;
12) silica content: 97.2 percent;
13) product pore volume: 1.14 ml/g.
In the case of the example 2, the following examples are given,
a production process of silicon dioxide for choline chloride carrier.
1200L of sodium silicate stock solution with the concentration of 1.6mol/L is added into a synthesis kettle, the stirring speed of the synthesis kettle is kept at 35rpm, steam is introduced, the temperature is raised to 60 ℃, a proper amount of process water is added, the concentration of the sodium silicate solution is adjusted to 0.15mol/L, 25% sulfuric acid is added at the speed of 2500L/h, the acid addition is stopped when the pH value of a reaction solution is 8.5, the time is about 16min, and the stage is a rapid seed crystal preparation process.
Then, after the temperature is increased to 85-90 ℃, 98 percent sulfuric acid and sodium silicate stock solution are added for 25min at the temperature at the flow rates of 100L/h and 1500L/h simultaneously, and the synthesis is a one-stage synthesis; and (3) increasing the stirring speed to 105rpm, increasing the temperature to 90-95 ℃, and adding 98% sulfuric acid and sodium silicate stock solution at the temperature at the flow rates of 150L/h and 2000L/h for 20min at the same time, thereby carrying out two-stage synthesis.
Stopping adding the sodium silicate stock solution, reducing the flow rate of 98% sulfuric acid to 90L/h at 90-95 ℃, reducing the flow rate to about 15min, and stopping adding acid when the pH value of the reaction solution reaches 4.1. And (3) after aging for 15min, pumping the dilute slurry into a filter, washing a filter cake by using process water when a large amount of filtrate does not flow out any more until the drainage conductivity is 11.0ms/cm, stopping washing, transferring the filter cake to a pulping machine, stirring to be in a better flowing state, detecting the solid content of the concentrated slurry to be 22.6 percent and the pH value to be 6.9, and pumping to a centrifugal spray drying tower by using a pressurizing pump.
Drying the concentrated slurry in a centrifugal spray drying tower, wherein the temperature of hot air is 450 ℃, the rotating speed of an atomizer is 9000rpm, the outlet temperature is controlled to be 125 +/-5 ℃, the negative pressure is-100 Pa, and the aperture of an atomizing nozzle is 12.0 mm; and (3) packaging the product by using a vacuum packaging machine, controlling the negative pressure of the packaging to be-100 Pa, and controlling the heating decrement of the product to be 4.0-5.0%, thus obtaining a final finished product.
The quality indexes of the silicon dioxide prepared in the production process of the embodiment are tested as follows:
1) (105 ℃/2h) heating loss: 4.7 percent;
2) DOA uptake: 3.0 ml/g;
3) bulk specific gravity: 0.19;
4) pass rate of 40 mesh: 95 percent;
5) the screen-passing rate of 40-80 meshes: 66 percent;
6) 80-120 mesh oversize: 28%;
7) 200 mesh undersize: 1 percent;
8) soluble salt content: 1.3 percent of
9) BET specific surface area: 165m2/g；
10) The iron content: 230 ppm;
11) heavy metal content (in pb): 5.0 ppm;
12) silica content: 98.1 percent;
13) product pore volume: 1.17 ml/g.
In the case of the example 3, the following examples are given,
a production process of silicon dioxide for choline chloride carrier.
1500L of sodium silicate stock solution with the concentration of 1.6mol/L is added into a synthesis kettle, the stirring speed of the synthesis kettle is kept at 105rpm, steam is introduced, the temperature is raised to 90 ℃, a proper amount of process water is added, the concentration of the sodium silicate is adjusted to 0.55mol/L, 25 percent sulfuric acid is added at the speed of 1250L/h-2500L/h, the acid addition is stopped when the pH value of reaction liquid is 11.0, the time is about 27min, and the stage is a high-temperature seed crystal preparation process.
Then 98 percent sulfuric acid and sodium silicate stock solution are added for 40min at the temperature of 87-93 ℃ and at the flow rates of 60L/h and 900L/h at the same time, and the synthesis is a first-stage synthesis; after aging for 10min, 98% sulfuric acid and sodium silicate stock solution are added at the same time at 150L/h and 2000L/h flow rate for 20min at the same temperature, which is a two-stage synthesis.
Stopping adding the sodium silicate stock solution, reducing the flow rate of 98 percent sulfuric acid to 90L/h, and stopping adding acid when the pH value of the reaction solution reaches 5.4 after 20 min. And after aging for 45min, pumping the dilute slurry into a filter, washing a filter cake by using process water when a large amount of filtrate does not flow out any more until the drainage conductivity is 8.0ms/cm, stopping washing, transferring the filter cake to a pulping machine, stirring to form a better flowing state, detecting that the solid content of the concentrated slurry is 24.3 percent, and the pH value is 6.7, and pumping to a centrifugal spray drying tower by using a pressurizing pump.
Drying the concentrated slurry in a centrifugal spray drying tower, wherein the temperature of inlet hot air is 490-500 ℃, the rotating speed of an atomizer is set to 10800rpm, the outlet temperature is controlled to be 118 +/-5 ℃, the negative pressure is-50 Pa, and the aperture of an atomizing nozzle is 8.0 mm; and (3) packaging the product by using a vacuum packaging machine, controlling the negative pressure of the packaging to be-100 Pa, and controlling the heating decrement of the product to be 4.0-5.0%, thus obtaining the final product.
The quality indexes of the silicon dioxide prepared in the production process of the embodiment are tested as follows:
1) (105 ℃/2h) heating loss: 3.9 percent;
2) DOA uptake: 2.85 ml/g;
3) bulk specific gravity: 0.245;
4) pass rate of 40 mesh: 99.2 percent;
5) the screen-passing rate of 40-80 meshes: 53 percent;
6) 80-120 mesh oversize: 42%;
7) 200 mesh undersize: 4.2 percent;
8) soluble salt content: 2.17 percent
9) BET specific surface area: 171m2/g；
10) The iron content: 290 ppm;
11) heavy metal content (in lead): 7.2 ppm;
12) silica content: 96.4 percent;
13) product pore volume: 0.98 ml/g.
In the case of the example 4, the following examples are given,
the embodiment discloses application of the silicon dioxide prepared by the preparation process in the embodiments 1-3 as a choline chloride carrier.
In the embodiment 1-3, a unique synthesis process is adopted in the synthesis stage of the semi-finished product, and sulfuric acid with different concentrations is used in different synthesis stages so as to ensure the large pore volume, high adsorbability and microstructure stability of the product; the four-stage synthesis process of adding sodium silicate three times and sulfuric acid four times is adopted to control the secondary structure of the product to be uniform without generating gel. The product is dried by adopting a centrifugal spray drying mode, particularly the size and the proper rotating speed of a nozzle in an atomizer are controlled, the narrower particle size distribution and the lower fine powder content of the product are ensured, and meanwhile, the flowability of the product is improved; the medium-low temperature drying ensures that the product surface generates rich gullies and wrinkles, has larger adsorption surface and unique surface microstructure, and is more beneficial to the adsorption of choline chloride; and the packaging link adopts vacuum negative pressure packaging, so that fine dust generated by mutual friction in product flowing is effectively removed. The comprehensive use of the technologies ensures that the produced silicon dioxide product has the characteristics of large adsorption proportion, excellent dispersibility and excellent fluidity after adsorbing choline chloride.
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, the technical solutions between the various embodiments can be combined with each other, but must be based on the realization of those skilled in the art; where combinations of features are mutually inconsistent or impractical, such combinations should not be considered as being absent and not within the scope of the claimed invention.
Claims (10)
1. A production process of silicon dioxide for choline chloride carrier is characterized by comprising the following steps,
s1: preparing seed crystals, namely adding sodium silicate stock solution into a synthesis kettle, wherein the modulus of the sodium silicate stock solution is 3.0-3.2, the concentration of the sodium silicate stock solution is 0.8-1.8 mol/L, introducing process steam under the stirring state of the synthesis kettle, heating to 40-60 ℃, adding process water to adjust the concentration of the liquid sodium silicate solution to 0.15-0.45 mol/L, adding sulfuric acid with the concentration of 15-30% into the reaction kettle at the speed of 1250-2500L/h, stopping adding acid when the pH of the reaction solution is 7.0-11.0, and keeping for 15-30 min;
s2: first-stage synthesis, namely raising the temperature to 60-90 ℃, keeping stirring, then adding 30-98% of sulfuric acid at the speed of 60-100L/h, and simultaneously adding the sodium silicate stock solution at the speed of 900-1500L/h, wherein the adding time of the two is 20-50 min;
s3: the second-stage synthesis, namely raising the temperature to 60-90 ℃, keeping stirring, adding 30-98% of sulfuric acid at the speed of 105-150L/h, and simultaneously adding the stock solution of sodium silicate at the speed of 1350-2000L/h, wherein the adding time of the two is 20-40 min;
s4: preparing a semi-finished product, namely adding 30-98% sulfuric acid at the speed of 45-90L/h at the temperature of the step S3 until the pH value of the reaction solution is 3.0-7.0, stopping adding acid, and aging for 30min under a stirring state to obtain a semi-finished product thin slurry;
s5: and (4) preparing a final product, namely filtering the semi-finished product thin slurry obtained in the step S4, washing, liquefying a filter cake, pulping, and drying by using a centrifugal spray drying tower to obtain the final product.
2. The production process of the silica for choline chloride carrier according to claim 1, wherein the process water has an electrical conductivity of 50 μ s/cm or less and a pH value of 7.0-7.5; the pressure of the steam for production is 0.5-1.0 MPa.
3. The process for producing silica for a choline chloride carrier according to claim 2, wherein the step S5 is performed by filtering with a box filter at a filtering pressure of 0.3 to 0.8MPa, washing with process water after filtering until the conductivity of washing water is 3.0 to 13.0ms/cm, transferring the filter cake to a pulper, and drying by pumping with a pressure pump when detecting that the solid content in the slurry is 15 to 25% while stirring to a flowing state.
4. The process for producing silica for a choline chloride carrier according to claim 1, wherein the stock solution of sodium silicate in step S1 is prepared by dissolving solid sodium silicate in process water and process steam in a dissolution kettle, wherein the stock solution of sodium silicate has a transparency of 5.0NTU or less, a soluble solid content of solid sodium silicate of 99% or more, an iron content of 0.02% or less, and a heavy metal content (in pb) of 30mg/kg or less.
5. The process for producing silica for a choline chloride carrier according to claim 1, wherein the sulfuric acid in step S1 to step S4 is prepared from raw sulfuric acid, the concentration of the raw sulfuric acid is 93-98%, the transparency is greater than or equal to 80mm, and the heavy metal content (in pb) is less than or equal to 50 mg/kg.
6. The production process of the silica for choline chloride carrier according to claim 1, wherein the stirring speed in the synthesis kettle is 15-105 rpm.
7. The production process of the silica for choline chloride carrier according to claim 1, wherein the temperature of hot air inlet of the centrifugal spray drying tower is 200-500 ℃, the temperature of the air outlet is 90-130 ℃, the pressure of the feed is 0.1-0.3 MPa, the rotation speed of the atomizer is 5000-11000 rpm, the aperture of the atomizing nozzle is 5-12 mm, and the internal pressure of the centrifugal spray drying tower is-150 Pa-50 Pa.
8. The process for producing silica for a choline chloride carrier according to claim 1, wherein the final product of the step S5 is packaged under vacuum and negative pressure after being screened to remove fine powder with a mesh size of more than 200 meshes.
9. The process for producing silica for a choline chloride carrier according to claim 8, wherein the packing machine pressure is-300 Pa to-100 Pa.
10. Use of the silica prepared according to any one of the preparation processes of claims 1 to 7 as a carrier for choline chloride.
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| RU2799206C1 (en) * | 2022-06-27 | 2023-07-04 | Общество С Ограниченной Ответственностью "Комета" | Method for production of amorphous silicon dioxide in granule form |
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