LEAKAGE-PREVENTING HIGH PERFORMANCE DESICCANT COMPOSITION AND PREPARATION METHOD THEREFOR
20230226517 · 2023-07-20
Assignee
Inventors
- Byeong Uk NAM (Asan-si, Chungcheongnam-do, KR)
- Jin Woo BAE (Gyeonggi-do, KR)
- Jong In LEE (Cheongju-si, Chungcheongbuk-do, KR)
Cpc classification
B01J20/28
PERFORMING OPERATIONS; TRANSPORTING
B01J20/24
PERFORMING OPERATIONS; TRANSPORTING
B01J20/30
PERFORMING OPERATIONS; TRANSPORTING
B01J20/04
PERFORMING OPERATIONS; TRANSPORTING
B01J20/046
PERFORMING OPERATIONS; TRANSPORTING
C09K3/18
CHEMISTRY; METALLURGY
B01J20/3085
PERFORMING OPERATIONS; TRANSPORTING
B01J20/26
PERFORMING OPERATIONS; TRANSPORTING
International classification
B01J20/04
PERFORMING OPERATIONS; TRANSPORTING
B01J20/24
PERFORMING OPERATIONS; TRANSPORTING
B01J20/28
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The present invention relates to a leakage-preventing high performance desiccant composition and a preparation method therefor, wherein a solid desiccant composition includes calcium chloride (CaCl.sub.2), magnesium chloride (MgCl.sub.2), and metal oxide, wherein the metal oxide may be calcium oxide (CaO), and a gel desiccant composition includes metal chloride and an absorbent polymer, wherein the metal chloride may be calcium chloride (CaCl.sub.2) and magnesium chloride (MgCl.sub.2), and the absorbent polymer may be CMC (carboxymethyl cellulose).
Claims
1. A solid desiccant composition comprising: calcium chloride (CaCl.sub.2)); magnesium chloride (MgCl.sub.2); and metal oxide.
2. The solid desiccant composition of claim 1, wherein a mass ratio of the calcium chloride and the magnesium chloride is 1:1 to 1:10.
3. The solid desiccant composition of claim 1, wherein a mass ratio of a sum of the calcium chloride and the magnesium chloride, and the metal oxide is 1:3 to 1:5.
4. A gel desiccant composition comprising: calcium chloride (CaCl.sub.2)); magnesium chloride (MgCl.sub.2); and an absorbent polymer.
5. The gel desiccant composition of claim 4, wherein the absorbent polymer is CMC (carboxymethyl cellulose).
6. The gel desiccant composition of claim 4, wherein a mass ratio of the calcium chloride and the magnesium chloride is 1:1 to 1:10.
7. The gel desiccant composition of claim 4, wherein a mass ratio of a sum of the calcium chloride and the magnesium chloride, and the absorbent polymer is 100:7.5 to 100:65.
8. A method of preparing a solid desiccant composition, the method comprising: mixing calcium chloride, magnesium chloride, and metal oxide to prepare a mixture; and subjecting metal oxide included in the mixture to a hydration reaction to generate metal hydroxide.
9. A method of preparing a gel desiccant composition, the method comprising: mixing calcium chloride, magnesium chloride, and an absorbent polymer to prepare a mixture; and forming a bond between metal cations of the calcium chloride and the magnesium chloride and hydrophilic anions of the absorbent polymer for gelation.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0017]
[0018]
[0019]
[0020]
MODE FOR CARRYING OUT THE INVENTION
[0021] Solid Desiccant Composition and Preparation Method Therefor
[0022] A solid desiccant composition according to an embodiment of the present invention includes calcium chloride (CaCl.sub.2), magnesium chloride (MgCl.sub.2), and metal oxide.
[0023] Calcium chloride (CaCl.sub.2) and magnesium chloride (MgCl.sub.2) may be prepared through various methods, and are not particularly limited. Calcium chloride (CaCl.sub.2) and magnesium chloride (MgCl.sub.2) have deliquescent properties that absorb moisture in the air (see
[0024] A mass ratio of the calcium chloride and the magnesium chloride may be 1:1 to 1:10, preferably 1:2.3 to 1:9.5, and most preferably 1:8.5 to 9.5. When calcium chloride is included in an excessively high amount, moisture absorption may decrease, and when magnesium chloride is included in an excessively high amount, preparation costs rise.
[0025] The metal oxide may be calcium oxide (CaO), magnesium oxide (MgO), or the like, but may preferably be calcium oxide (CaO). When magnesium oxide (MgO) is used, the curing rate is relatively slower than the curing rate shown when calcium oxide (CaO) is used, and some uncured materials may remain, leading to deterioration in quality. This may be prevented by using calcium oxide.
[0026] The metal oxide is mixed with calcium chloride (CaCl.sub.2) and magnesium chloride (MgCl.sub.2) to serve to form the mixture into a solid, and may prevent leakage.
[0027] A mass ratio of a sum of the calcium chloride and the magnesium chloride, and the metal oxide may be 1:0.5 to 1:4, more preferably 1:0.5 to 1:2. When metal oxide is included in an excessively low amount, solidification may not be performed well or leakage may be less prevented. When metal oxide is in an excessively high amount, moisture absorption may decrease.
[0028] A method of preparing a solid desiccant composition according to an embodiment of the present invention includes mixing calcium chloride, magnesium chloride, and metal oxide to prepare a mixture, and subjecting metal oxide included in the mixture to a hydration reaction to generate metal hydroxide.
[0029] In this case, descriptions of calcium chloride, magnesium chloride, and metal oxide may be the same as those described above.
[0030] In the preparing of the mixture, the mixing method is not particularly limited as long as calcium chloride, magnesium chloride, and metal oxide are mixed to be uniformly dispersed.
[0031] In the subjecting of metal oxide included in the mixture to a hydration reaction to generate metal hydroxide, the metal oxide may be formed into metal hydroxide through a hydration reaction by water absorbed by calcium chloride and magnesium chloride.
[0032] In this step, the mixture may be solidified by contacting moisture in the air with calcium chloride and magnesium chloride and subjecting the absorbed moisture and the metal oxide to a hydration reaction in a high-temperature atmosphere. Specifically, calcium chloride and magnesium chloride absorb moisture to generate calcium chloride hydrate CaCl.sub.2.Math.H.sub.2O and magnesium chloride hydrate MgCl.sub.2.Math.H.sub.2O, respectively. Metal oxide such as calcium oxide reacts with H.sub.2O of calcium chloride hydrate and magnesium chloride hydrate to generate calcium hydroxide (Ca(OH).sub.2) (see
[0033] The step herein may be performed in an atmosphere of constant humidity and temperature. Humidity may be set in the range of 80 to 95% RH and at a temperature of 40 to 60° C. This may lead to stable solidification to prevent generation of residues or breakage of products.
[0034] Gel Desiccant Composition and Preparation Method Therefor
[0035] A gel desiccant composition according to an embodiment of the present invention includes calcium chloride (CaCl.sub.2), magnesium chloride (MgCl.sub.2), and an absorbent polymer.
[0036] Descriptions of Calcium chloride (CaCl.sub.2) and magnesium chloride (MgCl.sub.2) may be the same as those described above.
[0037] A mass ratio of the calcium chloride and the magnesium chloride may be 1:1 to 1:10, preferably 1:2.3 to 1:9.5, and most preferably 1:8.5 to 9.5. When calcium chloride is included in an excessively high amount, moisture absorption may decrease, and when the content of magnesium chloride is included in an excessively high amount, preparation costs rise.
[0038] The absorbent polymer may form a three-dimensional network structure to absorb moisture into the network structure through capillarity and osmotic pressure. The absorbent polymer may include hydrophilic anions, for example, COO.sup.−, absorb a large amount of moisture through expanded space inside the network due to repulsive force between the anions, and form an ionic crosslinking reaction with calcium chloride and magnesium chloride to be subjected to gelation, thereby preventing leakage.
[0039] The absorbent polymer may preferably be CMC (Carboxymethyl cellulose). In this case, the CMC may be represented by Formula 1 below.
##STR00001##
[0040] A mass ratio of a sum of the calcium chloride and the magnesium chloride and the absorbent polymer may be 100:7.5 to 100:65, preferably 100:25 to 100:65, and more preferably 100:55 to 100:65. When the absorbent polymer is included in a small amount, viscosity decreases and thus leakage is less prevented, and when the absorbent polymer is included in an excessively large amount, moisture absorption may decrease.
[0041] A method of preparing a gel desiccant composition according to an embodiment of the present invention includes mixing calcium chloride, magnesium chloride, and an absorbent polymer to prepare a mixture, and forming a bond between metal cations of the calcium chloride and the magnesium chloride and hydrophilic anions of the absorbent polymer for gelation.
[0042] In this case, descriptions of calcium chloride, magnesium chloride, and an absorbent polymer may be the same as those described above.
[0043] In the preparing of the mixture, the mixing method is not particularly limited as long as calcium chloride, magnesium chloride, and an absorbent polymer are mixed to be uniformly dispersed.
[0044] The absorbent polymer may be CMC (Carboxymethyl cellulose), and in the preparing of the mixture, a mass ratio of the calcium chloride and magnesium chloride may be 1:2 to 1:10, preferably 1:2.3 to 1:9. In addition, a mass ratio of a sum of the calcium chloride and the magnesium chloride and the absorbent polymer may be 100:7.5 to 100:65, preferably 100:25 to 100:65, and more preferably 100:55 to 100:65.
[0045] Referring to
[0046] To this end, the step herein may include maintaining the temperature of a mixture to be 40 to 60° C. In this temperature range, crosslinking may be optimal. In addition, humidity may be maintained at 80 to 95% RH.
[0047] Determination of Moisture Absorption and Viscosity
[0048] Moisture absorption of a solid desiccant and a gel desiccant was obtained through the following formula after an initial weight of a sample, and a weight of a sample after reacting with moisture are determined.
Moisture absorption (%)=((W.sub.1−W.sub.0)/W.sub.0)×100
[0049] W.sub.0: Weight of sample before reaction with moisture
[0050] W.sub.1: Weight of sample after reaction with moisture
[0051] Viscosity of a gel desiccant was determined at 25° C. and 100 rpm, using a Brookfield viscometer.
Example 1
[0052] 0.5 g of calcium chloride and 4.5 g of magnesium chloride were mixed and weighed, and then the mixture was placed in a thermo-hygrostat and kept at 50° C. and 90% RH for 120 hours to react with moisture, and then the resulting product was weighed to determine moisture absorption.
Example 2
[0053] Moisture absorption was determined in the same manner as in Example 1, except that 1.5 g of calcium chloride and 3.5 g of magnesium chloride were mixed.
Example 3
[0054] Moisture absorption was determined in the same manner as in Example 1, except that 2.5 g of calcium chloride and 2.5 g of magnesium chloride were mixed.
Example 4
[0055] Moisture absorption was determined in the same manner as in Example 1, except that 3.5 g of calcium chloride and 1.5 g of magnesium chloride were mixed.
Example 5
[0056] Moisture absorption was determined in the same manner as in Example 1, except that 4.5 g of calcium chloride and 0.5 g of magnesium chloride were mixed.
Comparative Example 1
[0057] Moisture absorption was determined in the same manner as in Example 1, except that 5 g of calcium chloride was used alone without magnesium chloride.
Comparative Example 2
[0058] Moisture absorption was determined in the same manner as in Example 1, except that 10 g of calcium chloride was used alone without magnesium chloride.
Comparative Example 3
[0059] Moisture absorption was determined in the same manner as in Example 1, except that 20 g of calcium chloride was used alone without magnesium chloride.
Comparative Example 4
[0060] Moisture absorption was determined in the same manner as in Example 1, except that 40 g of calcium chloride was used alone without magnesium chloride.
Comparative Example 5
[0061] Moisture absorption was determined in the same manner as in Example 1, except that 5 g of magnesium chloride was used alone without calcium chloride.
Comparative Example 6
[0062] Moisture absorption was determined in the same manner as in Example 1, except that 10 g of magnesium chloride was used alone without calcium chloride.
Comparative Example 7
[0063] Moisture absorption was determined in the same manner as in Example 1, except that 20 g of magnesium chloride was used alone without calcium chloride.
Comparative Example 8
[0064] Moisture absorption was determined in the same manner as in Example 1, except that 40 g of magnesium chloride was used alone without calcium chloride.
[0065] The moisture absorption of Examples 1 to 5 and Comparative Examples 1 to 8 is shown in Table 1 below.
TABLE-US-00001 TABLE 1 Calcium Magnesium Moisture chloride chloride absorption (g) (g) (%) Example 1 0.5 4.5 473 Example 2 1.5 3.5 454 Example 3 2.5 2.5 438 Example 4 3.5 1.5 425 Example 5 4.5 0.5 412 Comparative 5 0 394 Example 1 Comparative 10 0 408 Example 2 Comparative 20 0 416 Example 3 Comparative 40 0 420 Example 4 Comparative 0 5 410 Example 5 Comparative 0 10 425 Example 6 Comparative 0 20 442 Example 7 Comparative 0 40 460 Example 8
[0066] Comparing Examples 1 to 5 measured using 5 g of a mixture of calcium chloride and magnesium chloride, Comparative Example 1 measured using only 5 g of calcium chloride, and Comparative Example 5 measured using only 5 g of magnesium chloride, it is seen that the moisture absorptions when calcium chloride and magnesium chloride are mixed are all high. In particular, when a mass ratio of calcium chloride and magnesium chloride is 1:1 to 1:9 (Examples 1 to 3), it is seen that the moisture absorption is significantly higher than the moisture absorptions of Comparative Examples 1 and 5.
[0067] Preparation of Solid Desiccant
[0068] Calcium oxide was added to calcium chloride and/or magnesium chloride to prepare solid desiccants whose moisture absorption was then determined for each.
Example 6
[0069] A mixture of 0.5 g of calcium chloride, 4.5 g of magnesium chloride, and 20 g of calcium oxide was prepared and weighed. Thereafter, the mixture was placed in a thermo-hygrostat and kept at 50° C. and 90% RH for 120 hours to prepare a solid desiccant, which was then weighed.
Example 7
[0070] A solid desiccant was prepared in the same manner as in Example 1, except that 1 g of calcium chloride, 9 g of magnesium chloride, and 20 g of calcium oxide were added upon preparing a mixture.
Example 8
[0071] A solid desiccant was prepared in the same manner as in Example 1, except that 2 g of calcium chloride, 18 g of magnesium chloride, and 20 g of calcium oxide were added upon preparing a mixture.
Example 9
[0072] A solid desiccant was prepared in the same manner as in Example 1, except that 4 g of calcium chloride, 36 g of magnesium chloride, and 20 g of calcium oxide were added upon preparing a mixture.
Comparative Example 9
[0073] A solid desiccant was prepared in the same manner as in Example 1, except that only 5 g of calcium chloride and 20 g of calcium oxide were used without magnesium chloride upon preparing a mixture.
Comparative Example 10
[0074] A solid desiccant was prepared in the same manner as in Example 1, except that only 10 g of calcium chloride and 20 g of calcium oxide were used without magnesium chloride upon preparing a mixture.
Comparative Example 11
[0075] A solid desiccant was prepared in the same manner as in Example 1, except that only 20 g of calcium chloride and 20 g of calcium oxide were used without magnesium chloride upon preparing a mixture.
Comparative Example 12
[0076] A solid desiccant was prepared in the same manner as in Example 1, except that only 40 g of calcium chloride and 20 g of calcium oxide were used without magnesium chloride upon preparing a mixture.
Comparative Example 13
[0077] A solid desiccant was prepared in the same manner as in Example 1, except that only 5 g of magnesium chloride and 20 g of calcium oxide were used without calcium chloride upon preparing a mixture.
Comparative Example 14
[0078] A solid desiccant was prepared in the same manner as in Example 1, except that only 10 g of magnesium chloride and 20 g of calcium oxide were used without calcium chloride upon preparing a mixture.
Comparative Example 15
[0079] A solid desiccant was prepared in the same manner as in Example 1, except that only 20 g of magnesium chloride and 20 g of calcium oxide were used without calcium chloride upon preparing a mixture.
Comparative Example 16
[0080] A solid desiccant was prepared in the same manner as in Example 1, except that only 40 g of magnesium chloride and 20 g of calcium oxide were used without calcium chloride upon preparing a mixture.
[0081] The moisture absorption of Examples 6 to 9 and Comparative Examples 9 to 16 is shown in Table 2 below.
TABLE-US-00002 TABLE 2 Calcium Magnesium Moisture chloride chloride Calcium absorption (g) (g) oxide (g) (%) Example 6 0.5 4.5 20 254 Example 7 1 9 20 312 Example 8 2 18 20 330 Example 9 4 36 20 368 Comparative 5 0 20 187 Example 9 Comparative 10 0 20 219 Example 10 Comparative 20 0 20 240 Example 11 Comparative 40 0 20 276 Example 12 Comparative 0 5 20 210 Example 13 Comparative 0 10 20 247 Example 14 Comparative 0 20 20 270 Example 15 Comparative 0 40 20 308 Example 16
[0082] Comparing Examples 6 to 9 with Comparative Examples 9 to 16, it is seen that when a total amount of calcium chloride and/or magnesium chloride is at the same level, Examples have high moisture absorption.
[0083] Preparation of Gel Desiccant
[0084] Absorbent polymers were added to calcium chloride and/or magnesium chloride to prepare gel desiccants whose moisture absorption was then determined for each.
Example 10
[0085] 0.5 g of calcium chloride, 4.5 g of magnesium chloride, and 3 g of CMC were mixed to prepare a mixture, which was then weighed, and then the mixture was placed in a thermo-hygrostat and kept at 50° C. and 90% RH for 120 hours to react with moisture, and then the resulting product was weighed to determine moisture absorption.
Example 11
[0086] Moisture absorption was determined in the same manner as in Example 10, except that 1 g of calcium chloride, 9 g of magnesium chloride, and 3 g of CMC were mixed upon preparing a mixture.
Example 12
[0087] Moisture absorption was determined in the same manner as in Example 10, except that 2 g of calcium chloride, 18 g of magnesium chloride, and 3 g of CMC were mixed upon preparing a mixture.
Example 13
[0088] Moisture absorption was determined in the same manner as in Example 10, except that 4 g of calcium chloride, 36 g of magnesium chloride, and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 17
[0089] Moisture absorption was determined in the same manner as in Example 10, except that 5 g of calcium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 18
[0090] Moisture absorption was determined in the same manner as in Example 10, except that 10 g of calcium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 19
[0091] Moisture absorption was determined in the same manner as in Example 10, except that 20 g of calcium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 20
[0092] Moisture absorption was determined in the same manner as in Example 10, except that 40 g of calcium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 21
[0093] Moisture absorption was determined in the same manner as in Example 10, except that 5 g of magnesium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 22
[0094] Moisture absorption was determined in the same manner as in Example 10, except that 10 g of magnesium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 23
[0095] Moisture absorption was determined in the same manner as in Example 10, except that 20 g of magnesium chloride and 3 g of CMC were mixed upon preparing a mixture.
Comparative Example 24
[0096] Moisture absorption was determined in the same manner as in Example 10, except that 40 g of magnesium chloride and 3 g of CMC were mixed upon preparing a mixture.
[0097] The moisture absorption of Examples 10 to 13 and Comparative Examples 17 to 24 is shown in Table 2 below.
TABLE-US-00003 TABLE 3 Calcium Magnesium Moisture chloride chloride CMC absorption Viscosity (g) (g) (g) (%) (cps) Example 10 0.5 4.5 3 420 47300 Example 11 1 9 3 443 25900 Example 12 2 18 3 463 14200 Example 13 4 36 3 487 6900 Comparative 5 0 3 365 46900 Example 17 Comparative 10 0 3 382 24800 Example 18 Comparative 20 0 3 402 13100 Example 19 Comparative 40 0 3 414 7800 Example 20 Comparative 0 5 3 376 45400 Example 21 Comparative 0 10 3 397 23700 Example 22 Comparative 0 20 3 423 12400 Example 23 Comparative 0 40 3 442 7000 Example 24
[0098] Comparing Examples 10 to 13 with Comparative Examples 17 to 24, it is seen that when a total amount of calcium chloride and/or magnesium chloride is at the same level, Examples have high moisture absorption.
[0099] In addition, in the case of Examples 10 and 11, when a total amount of calcium chloride and/or magnesium chloride is at the same level, Examples have a viscosity of 25000 or more, and accordingly, it is seen that the gel desiccant is stably prepared.
[0100] Desiccants were prepared as follows to observe changes in moisture absorption and viscosity according to the amount of an absorbent polymer.
Example 14
[0101] Moisture absorption was determined in the same manner as in Example 10, except that 0.5 g of calcium chloride, 4.5 g of magnesium chloride, and 1 g of CMC were mixed upon preparing a mixture.
Comparative Example 25
[0102] Moisture absorption was determined in the same manner as in Example 10, except that 0.5 g of calcium chloride, 4.5 g of magnesium chloride, and 5 g of CMC were mixed upon preparing a mixture.
Comparative Example 26
[0103] Moisture absorption was determined in the same manner as in Example 10, except that 0.5 g of calcium chloride, 4.5 g of magnesium chloride, and 10 g of CMC were mixed upon preparing a mixture.
[0104] The moisture absorption and viscosity of Examples 10 and 14 and Comparative Examples 25 and 26 are shown in Table 3 below.
TABLE-US-00004 TABLE 4 Calcium Magnesium Moisture chloride chloride CMC absorption Viscosity (g) (g) (g) (%) (cps) Example 14 0.5 4.5 1 445 16100 Example 10 0.5 4.5 3 420 47300 Comparative 0.5 4.5 5 387 — Example 25 Comparative 0.5 4.5 10 326 — Example 26
[0105] When it comes to the moisture absorption and viscosity of Examples 10 and 14 and Comparative Examples 25 and 26, Comparative Examples 25 and 26 having a high amount of an absorbent polymer may have a quite high viscosity, but have a rapidly decreasing moisture absorption of less than 400%. Meanwhile, it is seen that Example 14 having a small amount of an absorbent polymer has high moisture absorption and goes through gelation. Example 10, in which a mass ratio of a sum of calcium chloride and magnesium chloride and an absorbent polymer is 100:55 to 100:66, has a viscosity of 40000 or more and has a moisture absorption of 400% or more, indicating the best gel desiccant.