CN114249332A - Anti-caking boric acid treatment method and system - Google Patents
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Abstract
In order to solve the problem of serious agglomeration of the existing boric acid storage, the invention provides an anti-agglomeration boric acid treatment method, which comprises the following operation steps: dissolving a boric acid raw material in a solvent, fully dissolving, cooling and crystallizing to obtain a boric acid crystal mixed liquid, carrying out solid-liquid separation on the boric acid crystal mixed liquid to obtain a boric acid intermediate, and screening out more than 80% of the boric acid intermediate with the mesh number larger than 60 to obtain the anti-caking boric acid. The invention also provides an anti-caking boric acid treatment system. In the method for treating the anti-caking boric acid, the problem that the boric acid is seriously caked when stored can be well solved.
Description
Technical Field
The invention belongs to the technical field of boric acid purification, and particularly relates to an anti-caking boric acid treatment method and system.
Background
The industrial boric acid is prepared by processing and crystallizing boron-containing minerals by a sulfuric acid method, a hydrochloric acid method, a carbon ammonia method, a nitric acid method and the like, and the content of the boric acid can reach more than 95%. With the development of modern industry, the application field of boric acid is continuously widened, the product performance and quality requirements of the application field are gradually improved, and researches on refining and purifying boric acid and related industries are generated.
Boric acid makes the crystal surface wet and recrystallized due to the influence of the crystal itself, such as the property, chemical composition, crystal form, particle size distribution and crystal geometry, and external factors, such as humidity, temperature, pressure and impurities, etc., so that crystal bridges are formed at the mutual contact points between the crystal grains, and the crystal bridges make the crystal grains bonded together to gradually form huge lumps. At present, the boric acid in various application fields has the requirements of high purity, small bag packaging, quick dissolution and the like, and the industrial boric acid is produced by mainly adopting a recrystallization method and an ion exchange method in consideration of the cost and quality requirements. Although the recrystallization method and the ion exchange method have the advantages of simple flow, short time consumption, low cost and the like, the method has the problem of serious caking of boric acid after the boric acid is stored for a period of time.
Disclosure of Invention
Aiming at the problem that the existing boric acid can be seriously agglomerated during storage, the invention provides an anti-agglomeration boric acid treatment method and system.
The technical scheme adopted by the invention for solving the problems is as follows:
in a first aspect, the invention provides an anti-caking boric acid treatment method, which comprises the following operation steps:
dissolving a boric acid raw material in a solvent, fully dissolving, cooling and crystallizing to obtain a boric acid crystal mixed solution;
carrying out solid-liquid separation on the mixed liquid of the boric acid crystal to obtain a boric acid intermediate;
and screening the boric acid intermediate to remove 80% or more of the boric acid intermediate with the mesh number larger than 60 to obtain the anti-caking boric acid.
Optionally, in the screening operation, 92% or more of the boric acid intermediates having a mesh number greater than 60 are screened out.
Optionally, the step of performing solid-liquid separation on the mixed liquid of the boric acid crystal to obtain the boric acid intermediate comprises:
centrifuging the mixed liquid of the boric acid crystal to obtain a boric acid wet base;
and drying the boric acid wet base to obtain the boric acid intermediate.
Optionally, in the centrifugal operation, the percentage mass content of the crystals in the boric acid wet base is controlled to be 95.7% or more.
Optionally, in the drying operation, the percentage mass content of boric acid in the boric acid intermediate is controlled to be 99.30% or more.
Optionally, after "obtaining the boronic acid intermediate", the method further comprises:
and (4) carrying out compressed gas purging on the boric acid intermediate, and sealing and packaging after purging.
Optionally, the solvent is water, and the feeding ratio of the boric acid raw material to the water is (2-3.5): 1.
On the other hand, the invention also provides an anti-caking boric acid treatment system, which comprises a dissolving device, a crystallizing device, a centrifuging device, a drying device and a screening device;
the dissolving device is used for fully dissolving the added boric acid raw material in a solvent;
the crystallization equipment is used for cooling and crystallizing the dissolved boric acid raw material to obtain boric acid crystal mixed liquid;
the centrifugal equipment is used for carrying out solid-liquid separation on the boric acid crystal mixed liquid, and drying the boric acid crystal mixed liquid by the drying equipment to obtain a boric acid intermediate;
the screening equipment is used for screening the boric acid intermediates to screen out 80% or more of the boric acid intermediates with the mesh number larger than 60 so as to obtain the anti-caking boric acid.
Optionally, the system further comprises a cooling device, a bin and a packaging device;
the cooling device is used for cooling the boric acid intermediate;
the storage bin is used for storing and distributing the anti-caking boric acid, and the packaging equipment is used for sealing and packaging the anti-caking boric acid.
The inventor surprisingly finds that the boric acid intermediate is easy to agglomerate when the mesh number of the boric acid intermediate particles is larger, 80% or more of the boric acid intermediate with the mesh number larger than 60 is removed by screening, and the proportion of fine crystal particles in the boric acid is reduced, so that the anti-agglomeration boric acid can well prevent the boric acid from being stored and agglomerated.
Drawings
FIG. 1 is a process flow diagram provided by the present invention;
FIG. 2 is a graph showing the tendency of the average caking score of the ratio of boric acid of > 60 mesh to the content of the boric acid intermediate in example 1 and comparative example 1 provided by the present invention;
FIG. 3 is a graph showing the tendency of the average caking score in the content ratio of boric acid to boric acid intermediate of example 3 and comparative example 3 provided by the present invention.
The reference numbers in the drawings of the specification are as follows:
1. a dissolving device; 2. a crystallization device; 3. a centrifugal device; 4. a drying device; 5. a cooling device; 6. screening equipment; 7. a storage bin; 8. and (4) packaging equipment.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides an anti-caking boric acid treatment method, which comprises the following operation steps:
dissolving a boric acid raw material in a solvent, fully dissolving, cooling and crystallizing to obtain a boric acid crystal mixed solution;
carrying out solid-liquid separation on the mixed liquid of the boric acid crystal to obtain a boric acid intermediate;
and screening the boric acid intermediate to remove 80% or more of the boric acid intermediate with the mesh number larger than 60 to obtain the anti-caking boric acid.
The inventor surprisingly finds that the boric acid intermediate is easy to agglomerate when the mesh number of the boric acid intermediate particles is larger, 80% or more of the boric acid intermediate with the mesh number larger than 60 is removed by screening, and the proportion of fine crystal particles in the boric acid is reduced, so that the anti-agglomeration boric acid can well prevent the boric acid from being stored and agglomerated.
And cooling and crystallizing in the obtained boric acid crystal mixed liquid, wherein the stirring frequency can be controlled at 30-50Hz, the intermittent operation is adopted, and the cooling speed is controlled at 5-25 ℃/H. Cooling to less than or equal to 50 ℃ according to the boric acid solubility curve, the yield and the use condition of a mother liquor circulating system, and discharging and centrifuging.
In some embodiments of the invention, 92% and more of the boronic acid intermediates are screened out in a screening operation with a mesh size greater than 60.
In some embodiments of the present invention, the "performing solid-liquid separation on the mixed liquid of boric acid crystals to obtain a boric acid intermediate" includes:
centrifuging the mixed liquid of the boric acid crystal to obtain a boric acid wet base;
and drying the boric acid wet base to obtain the boric acid intermediate.
The mixed liquid of the boric acid crystal is centrifugally separated into solid and liquid, and the mother liquid can be discarded or conveyed to a mother liquid circulating system. The moisture in the boric acid wet base exists in the form of a boric acid saturated aqueous solution (mother liquor). The inventor finds that after drying, the mother liquor loses water, a crystallization process cannot be stably formed, and a large number of crystal clusters are formed on the surface of the crystal, so that the boric acid is crystallized regularly. The crystal clusters can wrap more intercrystalline moisture, and crystal bridges are more easily formed during storage, so that the crystal clusters are easy to agglomerate. Therefore, the aim of preventing caking can be effectively fulfilled by controlling the content of the moisture in the wet base.
In some embodiments of the invention, the percentage mass content of crystals in the boric acid wet base is controlled to be 95.7% and above in the centrifuging operation.
In order to further obtain the boric acid with better anti-caking performance, the content of the crystal in the boric acid wet base is controlled to be 95.7 percent or more.
In some preferred embodiments of the present invention, the percentage mass content of crystals in the boric acid wet base is controlled to 97.9% and above in the centrifugal operation.
In some embodiments of the present invention, the percentage mass content of boric acid in the boric acid intermediate is controlled to 99.30% by mass or more in the drying operation.
In order to further obtain the boric acid with better anti-caking performance, the percentage mass content of the boric acid in the boric acid intermediate is controlled to be 99.30 percent or more.
In some embodiments of the present invention, the percentage mass content of boric acid in the boric acid intermediate is controlled to 99.70% by mass or more in the drying operation.
In some embodiments of the present invention, after "obtaining the boronic acid intermediate", further comprising:
and (4) carrying out compressed gas purging on the boric acid intermediate, and sealing and packaging after purging.
Compressed gas is blown or blown into the boric acid intermediate, so that the temperature in the package can be reduced on one hand, and the aim of dehumidification is achieved on the other hand, thereby reducing the moisture among boric acid crystal grains and recrystallization in crystal bridges and preventing agglomeration.
In some embodiments of the present invention, the solvent is water, and the charge ratio of the boric acid raw material to water is (2-3.5): 1.
As shown in fig. 1, the invention further provides an anti-caking boric acid treatment system, which is characterized by comprising a dissolving device 1, a crystallizing device 2, a centrifugal device 3, a drying device 4 and a screening device 6, wherein the dissolving device 1 is used for fully dissolving an added boric acid raw material in a solvent, the crystallizing device 2 is used for cooling and crystallizing the dissolved boric acid raw material to obtain a boric acid crystal mixed solution, the centrifugal device 3 is used for carrying out solid-liquid separation on the boric acid crystal mixed solution, and a boric acid intermediate is obtained after the boric acid crystal mixed solution is dried by the drying device 4; the screening equipment 6 is used for screening the boric acid intermediates to screen out 80% or more of the boric acid intermediates with the mesh number larger than 60 so as to obtain the anti-caking boric acid.
In some embodiments of the invention, the system further comprises a cooling device 5, a silo 7 and a packaging device 8; the cooling device 5 is used for cooling the boric acid intermediate, and the storage bin 7 is used for storing and distributing the anti-caking boric acid and hermetically packaging the anti-caking boric acid by the packaging device 8.
In some embodiments of the present invention, the dissolving device 1 is a dissolving kettle, the crystallizing device 2 is a crystallizing kettle, the centrifuging device 3 is a centrifuge, the drying device 4 is a disc dryer, a rotary dryer, a rake dryer or a fluidized bed, the cooling device 5 is a rotary dryer, a paddle cooler or a fluidized bed, the screening device 6 is a vibrating screen, the packaging device 8 is a packaging machine, and the dehumidifying device includes a dehumidifier, an ice maker and a fan, and is used for introducing compressed air or nitrogen.
The present invention will be further illustrated by the following examples. It is to be understood that the present invention is not limited to the following embodiments, and methods are regarded as conventional methods unless otherwise specified. Materials are commercially available from the open literature unless otherwise specified.
Example 1
Example 1 is provided to illustrate the anti-caking boric acid treatment method disclosed in the present invention.
The anti-caking boric acid treatment method comprises the following steps:
1. putting boric acid raw materials and water into a 5000L dissolving kettle, wherein the feeding ratio of the boric acid raw materials to the water is (2-3.5):1, heating to 100 ℃ and pressurizing to dissolve;
2. transferring the materials to a crystallization kettle, stirring at the frequency of 30-50Hz, performing intermittent operation, and cooling at the cooling speed of 5-25 ℃/H to obtain a boric acid crystal mixed solution;
3. after the temperature is cooled to be less than or equal to 50 ℃, putting the mixed liquid of the boric acid crystal into a centrifuge for separating solid from liquid, and obtaining a boric acid wet base by changing the centrifugation time and the feeding ratio;
4. the boric acid wet base enters a disc type dryer for drying, and a boric acid intermediate is obtained through control;
5. introducing the boric acid intermediate into a double-paddle cooler, and controlling the temperature to be less than or equal to 50 ℃;
6. and transferring the boric acid intermediate to a vibrating screen for screening to remove 80% or more of the boric acid intermediate with the mesh number larger than 60, thereby obtaining the anti-caking boric acid.
Example 2
Example 2 is provided to explain the anti-caking boric acid treatment method disclosed in the present invention, including most of the operation steps in example 1, except that:
and (3) after the temperature is cooled to be less than or equal to 50 ℃, putting the mixed liquid of the boric acid crystals into a centrifugal machine to separate solid and liquid, and obtaining the boric acid wet base with the crystal content of 95.7 percent or more of the boric acid wet base content by changing the centrifugal time and the feed ratio.
Example 3
Example 3 is for explaining the anti-caking boric acid treatment method disclosed by the present invention, which comprises most of the operation steps of example 1, except that:
and (4) drying the boric acid wet base in a disc type dryer, and controlling to obtain a boric acid intermediate with the boric acid percentage mass content of 99.30% or more.
Example 4
Example 4 is provided to illustrate the anti-caking boric acid treatment method disclosed in the present invention, which comprises most of the steps of example 1, except that:
step (7) is further included after step (6), and step (7): the anti-caking boric acid enters a storage bin and is packaged in a packaging machine;
wherein, the 500KPa compressed air (or nitrogen) is used for purging and replacing in the steps (5) to (7).
Comparative example 1
Comparative example 1 for comparative illustration of the anti-caking boric acid treatment method disclosed in the present invention, comprising most of the operational steps of example 1, except that:
in the step (6), transferring the boric acid intermediate to a vibrating screen for screening, and screening out less than 80% of the boric acid intermediate with the mesh number larger than 60 to obtain the anti-caking boric acid.
Comparative example 2
Comparative example 2 for comparative illustration of the anti-caking boric acid treatment method disclosed in the present invention, comprising most of the operational steps of example 1, except that:
and (3) after the temperature is cooled to be less than or equal to 50 ℃, putting the mixed liquid of the boric acid crystals into a centrifugal machine to separate solid and liquid, and changing the centrifugal time and the feed ratio to obtain the boric acid wet base with the content of the crystals in the boric acid wet base being less than 95.7%.
Comparative example 3
Comparative example 3 for comparative illustration of the anti-caking boric acid treatment method disclosed in the present invention, comprising most of the operational steps of example 1, except that:
in the step (4), the boric acid wet base is circulated or enters a disc type dryer for drying, and the boric acid intermediate with the percentage mass content of less than 99.30 percent is obtained by controlling.
Performance scoring
Setting a grading standard: the boric acid product is placed in a warehouse for storage for 3 months, the caking degree of the product is scored (0-5 points), and the influence of factors on caking is judged according to the scores.
And 5, dividing: no caking and a quicksand shape;
and 4, dividing: slightly caking, i.e. crumbling to the touch;
and 3, dividing: slightly caking, and the powder is smashed by hand;
and 2, dividing: caking, namely, the caking is broken by lightly knocking with a mallet;
1 minute: if the caking is serious, the caking needs to be forcibly broken by a mallet;
0 minute: the boric acid in the whole bag is hardened due to severe caking, and the caking needs to be broken by force and is scattered into small caking.
First, in example 1, boric acid intermediates were finely sieved according to mesh size range to obtain groups of mesh size range 12-30 mesh, 30-40 mesh, 40-60 mesh and > 60 mesh, which were divided into 4 groups of 5 experiments each to obtain average clumping score as shown in table 1.
TABLE 1
As can be seen from Table 1, the smaller the mesh number of the boric acid intermediate, the larger the grain size, the less likely to agglomerate, and among them, the 12-30 mesh size was achieved, and the boric acid was free from agglomeration.
And secondly, dividing the boric acid into 12 groups and each group for 3 times of experiments according to different content ratios of the boric acid intermediates with boric acid of more than 60 meshes in the experiment to obtain average caking scores in the table 2, wherein the numbers 1 to 8 in the table 2 are the experimental groups with the proportion of the components with more than 60 meshes in the example 1, and the numbers 9 to 12 in the table 2 are the experimental groups with the proportion of the components with more than 60 meshes in the comparative example 1. And an average caking score trend graph as shown in fig. 2 was prepared according to the average caking score of table 2.
TABLE 2
As can be seen from Table 2 and FIG. 2, it is found that boric acid intermediates having a mesh number of 80% or more and larger than 60 are removed by screening, and storage caking of boric acid is preferably prevented, and boric acid intermediates having a mesh number of 92% or more and larger than 60 are removed by screening if boric acid having a better anti-caking property is to be obtained.
And thirdly, obtaining different boric acid wet basis contents by regulating and controlling the centrifugation time and the feeding ratio, dividing the boric acid wet basis contents into 18 groups, and performing 5 experiments on each group, and obtaining the average caking score shown in the table 3 after drying and storing at normal temperature for 3 months. Wherein, the numbers 1 to 12 in the table 3 are experimental groups of the crystal in the range of the boric acid wet basis content of the example 2, and the numbers 13 to 18 in the table 3 are experimental groups of the crystal in the range of the boric acid wet basis content of the comparative example 2.
TABLE 3
From the results shown in table 3, it is understood that the percentage mass content of the crystals in the boric acid wet base is controlled to 95.7% or more, which can prevent the boric acid from being stored and agglomerated well, and if the boric acid with better anti-agglomeration performance is to be obtained, the percentage mass content of the crystals in the boric acid wet base is controlled to 97.9% or more.
And fourthly, dividing the boric acid intermediate into 7 groups by controlling the percentage mass content (%) of boric acid in the boric acid intermediate, and performing a plurality of experiments to obtain the caking scores shown in the table 4. Wherein, numbers 4 to 7 of Table 4 are experimental groups within the range of the percentage mass content of boric acid in the boric acid intermediate of example 3, and numbers 1 to 3 of Table 4 are experimental groups within the range of the percentage mass content of boric acid in the boric acid intermediate of comparative example 3.
TABLE 4
An average caking score trend chart as shown in fig. 3 was prepared according to the percentage mass content ranges of boric acid shown in table 4.
As can be seen from table 4 and fig. 3, the percentage mass content of boric acid in the boric acid intermediate is controlled to 99.30% or more, which can prevent the boric acid from caking during storage. If boric acid with better anti-caking performance is obtained, the percentage mass content of the boric acid in the boric acid intermediate is controlled to be 99.70% or more.
Fifthly, comparative example 1 and example 4 were different in that 500KPa compressed air (or nitrogen) purge replacement was used in the steps (5) to (7) of example 4 and 500KPa compressed air (or nitrogen) purge replacement was not used in example 1, and the boric acid temperature for anti-blocking in the package, the relative humidity in the package and the blocking score were obtained as shown in table 5.
TABLE 5
As is clear from table 5, in comparative example 1 and example 4, the boric acid intermediate was subjected to the dehumidification treatment, so that the temperature in the package and the relative humidity in the bag of the package could be lowered, and the boric acid anti-caking property was improved.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The anti-caking boric acid treatment method is characterized by comprising the following operation steps:
dissolving a boric acid raw material in a solvent, fully dissolving, cooling and crystallizing to obtain a boric acid crystal mixed solution;
carrying out solid-liquid separation on the mixed liquid of the boric acid crystal to obtain a boric acid intermediate;
and screening the boric acid intermediate to remove 80% or more of the boric acid intermediate with the mesh number larger than 60 to obtain the anti-caking boric acid.
2. The method of claim 1, wherein 92% or more of the boric acid intermediates having a mesh size greater than 60 are removed by sieving.
3. The method of claim 1, wherein the step of subjecting the liquid mixture of boric acid crystals to solid-liquid separation to obtain a boric acid intermediate comprises:
centrifuging the mixed liquid of the boric acid crystal to obtain a boric acid wet base;
and drying the boric acid wet base to obtain the boric acid intermediate.
4. The method according to claim 3, wherein the percentage mass content of the crystals in the boric acid wet base is controlled to 95.7% by mass or more in the centrifugal operation.
5. The method according to claim 3, wherein the percentage mass content of boric acid in the boric acid intermediate is controlled to 99.30% by mass or more in the drying operation.
6. The method of claim 1, further comprising, after "obtaining the boronic acid intermediate":
and (4) carrying out compressed gas purging on the boric acid intermediate, and sealing and packaging after purging.
7. The method according to claim 1, wherein the solvent is water, and the charge ratio of the boric acid raw material to the water is (2-3.5): 1.
8. An anti-caking boric acid treatment system is characterized by comprising a dissolving device, a crystallizing device, a centrifuging device, a drying device and a screening device;
the dissolving device is used for fully dissolving the added boric acid raw material in a solvent;
the crystallization equipment is used for cooling and crystallizing the dissolved boric acid raw material to obtain boric acid crystal mixed liquid;
the centrifugal equipment is used for carrying out solid-liquid separation on the boric acid crystal mixed liquid, and drying the boric acid crystal mixed liquid by the drying equipment to obtain a boric acid intermediate;
the screening equipment is used for screening the boric acid intermediates to screen out 80% or more of the boric acid intermediates with the mesh number larger than 60 so as to obtain the anti-caking boric acid.
9. The anti-caking boric acid processing system of claim 8 further comprising a cooling apparatus, a silo and a packaging apparatus;
the cooling device is used for cooling the boric acid intermediate;
the storage bin is used for storing and distributing the anti-caking boric acid, and the packaging equipment is used for sealing and packaging the anti-caking boric acid.
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| CN102502711A (en) * | 2011-10-20 | 2012-06-20 | 中盐金坛盐化有限责任公司 | Preparation process and special device for salt with green food label |
| CN103787349A (en) * | 2012-10-31 | 2014-05-14 | 中国地质科学院矿产综合利用研究所 | Preparation method of nuclear-grade high-purity boric acid |
| CN104150499A (en) * | 2013-05-14 | 2014-11-19 | 中国地质科学院矿产综合利用研究所 | Preparation method of high-purity boric acid and nuclear grade high-purity boric acid |
| WO2016099095A1 (en) * | 2014-12-15 | 2016-06-23 | 오씨아이 주식회사 | Method for preparing agglomerated boron nitride powder |
| CN105236439A (en) * | 2015-09-07 | 2016-01-13 | 成都程德化工科技有限责任公司 | Large-granular boric acid, continuously cooling recrystallization preparation process and continuously cooling recrystallization preparation method thereof |
| CN105347353A (en) * | 2015-12-17 | 2016-02-24 | 丹东市化学试剂厂 | Preparation method of high-purity boric acid |
| CN106111532A (en) * | 2016-06-28 | 2016-11-16 | 四川省汉源化工总厂 | A kind of stage division of feed-level calcium biphosphate |
| CN108249453A (en) * | 2018-03-05 | 2018-07-06 | 西陇科学股份有限公司 | A kind of preparation of modification infusorial earth and its method for being used to prepare high-purity boracic acid |
| WO2019175824A1 (en) * | 2018-03-14 | 2019-09-19 | Tubitak | Purification of boric acid |
| CN110054196A (en) * | 2019-04-10 | 2019-07-26 | 大连理工大学 | The method that one organic molecular species induction prepares the instant boric acid of high pure spherical |
| CN110357127A (en) * | 2019-06-28 | 2019-10-22 | 孝感广盐华源制盐有限公司 | A kind of anti-caking eats the production method of sodium chloride |
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