CN112755741A - Color-changing gas drying agent and preparation method and application thereof - Google Patents
Color-changing gas drying agent and preparation method and application thereof Download PDFInfo
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- CN112755741A CN112755741A CN202011396104.0A CN202011396104A CN112755741A CN 112755741 A CN112755741 A CN 112755741A CN 202011396104 A CN202011396104 A CN 202011396104A CN 112755741 A CN112755741 A CN 112755741A
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- drying agent
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- gas
- desiccant
- changing gas
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- 239000002274 desiccant Substances 0.000 title claims abstract description 152
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000002245 particle Substances 0.000 claims abstract description 48
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 claims abstract description 38
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 32
- 238000000746 purification Methods 0.000 claims abstract description 13
- 238000004868 gas analysis Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 48
- 239000011259 mixed solution Substances 0.000 claims description 40
- 238000001291 vacuum drying Methods 0.000 claims description 26
- 230000018044 dehydration Effects 0.000 claims description 20
- 238000006297 dehydration reaction Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 9
- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 23
- 230000008859 change Effects 0.000 abstract description 11
- 239000007789 gas Substances 0.000 description 87
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920002749 Bacterial cellulose Polymers 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000005016 bacterial cellulose Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000010364 biochemical engineering Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/28—Selection of materials for use as drying agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/261—Drying gases or vapours by adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Drying Of Gases (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The invention relates to a color-changing gas drying agent and a preparation method and application thereof, wherein the color-changing gas drying agent comprises anhydrous magnesium perchlorate and cobalt chloride in a mass ratio of 98-99: 1-2, and the particle size of the drying agent is 2-4 mm. Compared with the prior art, the invention has the advantages of small air resistance, strong water absorption capacity, obvious color change, granular shape, convenient use, no volatile component, suitability for the field of gas analysis and purification and the like.
Description
Technical Field
The invention relates to the technical field of gas analysis and purification, in particular to a color-changing gas drying agent and a preparation method and application thereof.
Background
The desiccant is a water removal agent which absorbs moisture from the atmosphere, can effectively remove moisture and prevent damp, and adopts the principle that water molecules are absorbed in the self structure in a physical mode or absorbed in a chemical mode. The application range of the drying agent is quite wide, and the drying agent is required to be used for storage, circulation, storage, driving protection and navigation of products in the industrial production fields of medicine, electronics, machinery, metal products, glass, biochemical engineering and the like and the marine transportation process of containers. Some industrial gases often require dehydration refining during use: such as hydrogen, oxygen, nitrogen, chlorine, carbon dioxide, acetylene, ethylene, and the like.
At present, inorganic compounds with moisture absorption function, such as calcium chloride, calcium oxide, sodium sulfate, magnesium sulfate, sodium hydroxide and the like, as well as activated carbon, molecular sieves, silica gel, bentonite, attapulgite, polyamide and the like, which have certain moisture absorption capacity, are mainly used as the drying agent, but have the common defect that the drying agent has no capacity of directly indicating moisture absorption information, and a user cannot timely judge the effectiveness of moisture absorption and when the drying agent should be replaced in real time when using the drying agent.
The invention patent CN105170102A discloses a preparation method of a color-changing drying agent for gas, which comprises the following steps: after a specific culture medium is prepared, microbial fermentation is carried out to prepare bacterial cellulose microspheres containing nano activated carbon, and then the color-changing drying agent is prepared after modification, dip dyeing and drying. The drying agent prepared by the preparation method of the color-changing drying agent provided by the invention has the advantages of strong moisture absorption and retention capacity, obvious color change and the like. However, the preparation method of the drying agent is complex, the drying agent contains substances such as glucose, edible alcohol, yeast powder, pectin and nano active carbon, the edible alcohol belongs to volatile substances, and the substances such as the glucose, the yeast powder, the pectin and the nano active carbon are easy to generate fragments, which do not meet the requirements of gas analysis and gas purification.
The invention patent CN102658005B discloses a novel humidity-sensitive color-changing desiccant, which mainly comprises three components, namely a microcrystalline dye, a connecting material and a desiccant, wherein the mass ratio of the components is 0.01-5: 0.01-5: 90-99.98. The desiccant realizes color change indication by means of dissolution of the microcrystalline dye, and in a moisture environment, after the desiccant absorbs moisture, the moisture is conducted to the microcrystalline dye, so that the microcrystalline dye is dissolved and changes color. The invention senses the moisture through color change vision, and informs a user to replace a fresh drying agent in time along with the deepening of the color change color, thereby improving the moisture adsorption effect. However, the average particle size of the color-changing drying agent is 10-500 microns, the particle size is small, the air resistance is large, and the requirements of a gas analysis instrument cannot be met. The drying agent is one or more of molecular sieve, silica gel, alumina, aluminum hydroxide, attapulgite, bentonite, clay, diatomite, active carbon or polyamide, has low dehydration property, and cannot meet the requirements of gas analysis and gas purification.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a color-changing gas drying agent, a preparation method and application thereof, which have the advantages of strong water absorption capacity, strong color-developing indicating capacity, no volatile component and suitability for gas analysis and purification processes.
The purpose of the invention can be realized by the following technical scheme: a color-changing gas drying agent comprises anhydrous magnesium perchlorate and cobalt chloride in a mass ratio of 98-99: 1-2, and the particle size of the drying agent is 2-4 mm. The drying agent has larger grain diameter, no holes or cracks on the surface of the grains, small air resistance and difficult taking away by air flow.
The anhydrous magnesium perchlorate is a high-efficiency drying agent, has extremely strong water absorption capacity, and is used for preparing a deeply dehydrated drying agent. The anhydrous magnesium perchlorate is granular or powdery, has no corrosiveness and convenient use, but has the defect of unobvious color change after water absorption, and can not judge whether the anhydrous magnesium perchlorate is saturated and fails or not in time. Cobalt chloride is a red monoclinic crystal, is stable at room temperature, loses crystal water to turn blue when heated, and turns red in humid air. The anhydrous magnesium perchlorate and the cobalt chloride of the desiccant can reduce the residual water content of the dried gas to 1ppmv (-76 ℃ dew point) within the mass ratio range, show excellent hygroscopicity and can meet the requirements of gas analysis and gas purification. In addition, the anhydrous magnesium perchlorate and the cobalt chloride of the desiccant are changed into pink from blue after absorbing moisture in the mass ratio range, so that a user is reminded to replace the desiccant, the color difference before and after the color change is obvious and easy to identify, and the desiccant does not reach water absorption saturation far after changing into pink, so that the desiccant can be ensured to have excellent hygroscopicity in the normal use stage. And the drying agent can be heated and dried after being replaced, the drying performance of the drying agent is recovered again, the drying agent can be repeatedly used, and the cost of a user is reduced.
The preparation method of the color-changing gas desiccant comprises the following steps:
(1) uniformly mixing anhydrous magnesium perchlorate, cobalt chloride and water to prepare a mixed solution;
(2) removing water to obtain a large block of drying agent;
(3) crushing the large drying agent to obtain a small-particle drying agent;
(4) deeply dehydrating the small-particle drying agent to obtain the color-changing gas drying agent.
Further, the mass ratio of the anhydrous magnesium perchlorate, the cobalt chloride and the water in the step (1) is 98-99: 1-2: 120-150, the anhydrous magnesium perchlorate is dissolved in the water under stirring, and then the cobalt chloride is added.
Furthermore, the rotating speed in the stirring process is 300-600 rpm, the temperature is normal temperature, and the time is 0.5-1.0 h.
And (3) the moisture removing process in the step (2) is to place the mixed solution in an oven for heating dehydration, wherein the heating temperature is 150-180 ℃, and the heating time is 2-4 hours.
Furthermore, the water content of the bulk drying agent is 1-5%.
And (4) adopting a coarse crusher in the crushing process in the step (3).
The deep dehydration process in the step (4) is specifically as follows: and (3) placing the small-particle drying agent into a vacuum drying oven for vacuum heating dehydration, wherein the vacuum degree is-0.1 to-0.06 MPa, the heating temperature is 120 to 150 ℃, and the heating time is 1 to 3 hours.
The application of the color-changing gas drying agent is to apply the color-changing drying agent to the fields of gas analysis and gas purification.
Further, the gas comprises H2、O2、Cl2、HCl、NH3Or CO2。
The color-changing gas drying agent can be used as an ideal drying agent for domestic or imported infrared carbon, sulfur, hydrogen, oxygen, nitrogen and other gas analytical instruments, and is also suitable for a dehydrating agent for gas purification. In the using process, glass fiber can be used for fixing desiccant particles at the air inlet and the air outlet of the desiccant, so that the desiccant is prevented from being brought into an analysis instrument by airflow, and the requirements of a gas analysis instrument are met. The dew point of the gas purification is required to be lower than-65 ℃, and the drying agent of the invention can reduce the residual water content of the dried gas to 1ppmv (-76 ℃ dew point), thereby meeting the requirement of gas purification.
Compared with the prior art, the invention has the following advantages:
1. the color-changing gas desiccant has the advantages of obvious color change, strong water absorption capacity, small air resistance and no volatile component, and is suitable for the fields of gas analysis, gas purification and the like;
2. the color-changing gas drying agent is 2-4mm granular, is convenient to take and use, and is not easy to bring into an analysis or purification instrument by airflow;
3. the color difference before and after the color of the color-changing gas desiccant is obvious and easy to identify, and the desiccant does not reach water absorption saturation far after changing into pink, so that the desiccant can be ensured to have excellent hygroscopicity in a normal use stage;
4. the color-changing gas drying agent can be heated and dried after being replaced, the drying performance of the color-changing gas drying agent is recovered again, the color-changing gas drying agent can be repeatedly used, and the cost of a user is reduced.
Detailed Description
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 120.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 150 ℃ for 4 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08 MPa, the heating temperature is 120 ℃, and the heating time is 3 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for drying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 2
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 2:98: 120.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 150 ℃ for 4 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 120 ℃, and the heating time is 3 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for drying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 3
(1) Preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 120.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 120 ℃, and the heating time is 3 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for drying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 4
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 120.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 150 ℃ for 4 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 130 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for drying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 5
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 130.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 150 ℃ for 4 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 120 ℃, and the heating time is 3 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for purifying oxygen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 6
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 130.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 140 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for purifying oxygen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 7
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 150.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 180 ℃ for 2 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.1M Pa, the heating temperature is 140 ℃, and the heating time is 1 hour, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for purifying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Example 8
A preparation method of a color-changing gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:99: 150.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 180 ℃ for 2 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.06M Pa, the heating temperature is 150 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The discoloring gas desiccant is used for purifying hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point). The color-changing gas desiccant changes from blue to pink before and after water absorption.
Comparative example 1
A preparation method of a gas desiccant comprises the following steps:
(1) preparing a mixed solution of anhydrous magnesium perchlorate and water, wherein the mass ratio of the anhydrous magnesium perchlorate to the water is 99: 130.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 140 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The gas drying agent is used for drying the hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point), and the gas drying agent does not change color before and after water absorption.
Comparative example 2
A preparation method of a gas desiccant comprises the following steps:
(1) preparing a mixed solution of anhydrous magnesium perchlorate and water, wherein the mass ratio of the anhydrous magnesium perchlorate to the water is 99: 130.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 140 ℃, and the heating time is 2 hours, thus obtaining the gas drying agent.
The gas drying agent is used for drying the hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point), and the gas drying agent does not change color before and after water absorption.
Comparative example 3
A preparation method of a gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 1:101: 140.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 140 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The gas drying agent is used for drying the hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1ppmv (-76 ℃ dew point), and the gas drying agent changes color before and after absorbing water, but the color change is not obvious.
Comparative example 4
A preparation method of a gas desiccant comprises the following steps:
(1) preparing a mixed solution of cobalt chloride, anhydrous magnesium perchlorate and water, wherein the mass ratio of the cobalt chloride to the anhydrous magnesium perchlorate to the water is 3:97: 140.
(2) And (2) uniformly stirring the mixed solution obtained in the step (1), putting the mixed solution into a common oven, heating and dehydrating at the temperature of 160 ℃ for 3 hours, and crushing the obtained large drying agent into small particles with the particle size of 2-4 mm.
(3) And (3) putting the small-particle drying agent obtained in the step (2) into a vacuum drying oven for deep dehydration, so that the vacuum degree in the vacuum drying oven reaches-0.08M Pa, the heating temperature is 140 ℃, and the heating time is 2 hours, thus obtaining the color-changing gas drying agent.
The gas drying agent is used for drying the hydrogen with the water content of 1 percent, so that the residual water content of the dried gas can be reduced to 1.2ppmv, and the color-changing gas drying agent is changed from blue to pink before and after water absorption.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The color-changing gas drying agent is characterized by comprising anhydrous magnesium perchlorate and cobalt chloride in a mass ratio of 98-99: 1-2, wherein the particle size of the drying agent is 2-4 mm.
2. A method of preparing a colour-changing gas desiccant as claimed in claim 1, comprising the steps of:
(1) uniformly mixing anhydrous magnesium perchlorate, cobalt chloride and water to prepare a mixed solution;
(2) removing water to obtain a large block of drying agent;
(3) crushing the large drying agent to obtain a small-particle drying agent;
(4) deeply dehydrating the small-particle drying agent to obtain the color-changing gas drying agent.
3. The preparation method of the color-changing gas desiccant according to claim 2, wherein the mass ratio of the anhydrous magnesium perchlorate to the cobalt chloride to the water in the step (1) is 98-99: 1-2: 120-150, the anhydrous magnesium perchlorate is dissolved in the water under stirring, and then the cobalt chloride is added.
4. The method for preparing a desiccant for a color-changing gas as claimed in claim 3, wherein the rotation speed in the stirring process is 300-600 rpm, the temperature is normal temperature, and the time is 0.5-1.0 h.
5. The preparation method of the color-changing gas desiccant as claimed in claim 2, wherein the moisture removal process in the step (2) is to put the mixed solution into an oven for heating and dehydration, the heating temperature is 150-180 ℃, and the heating time is 2-4 h.
6. The method of claim 5, wherein the moisture content of the bulk desiccant is between 1% and 5%.
7. The method for preparing a color-changing gas desiccant as claimed in claim 2, wherein the pulverization in step (3) is carried out using a coarse pulverizer.
8. The method for preparing a color-changing gas desiccant as claimed in claim 2, wherein the deep dehydration process in step (4) is specifically as follows: and (3) placing the small-particle drying agent into a vacuum drying oven for vacuum heating dehydration, wherein the vacuum degree is-0.1 to-0.06 MPa, the heating temperature is 120 to 150 ℃, and the heating time is 1 to 3 hours.
9. Use of a colour-changing gas desiccant according to claim 1 in the field of gas analysis, gas purification.
10. The use of a color-changing gas desiccant as claimed in claim 9 wherein said gas comprises H2、O2、Cl2、HCl、NH3Or CO2。
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| CN1081393A (en) * | 1992-07-20 | 1994-02-02 | 中国科学院上海冶金研究所 | Highly effective drying agent and preparation method thereof |
| US20100248966A1 (en) * | 2005-01-07 | 2010-09-30 | Lynch James R | Homogeneous gas-evolving composition |
| CN105944553A (en) * | 2016-05-12 | 2016-09-21 | 张锐 | Quick waste gas desulphurization agent and preparation method thereof |
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| CN86101504A (en) * | 1986-06-26 | 1987-09-02 | 中国科学院上海冶金研究所 | High efficiency drier self-indicating |
| CN1044232A (en) * | 1988-06-18 | 1990-08-01 | 李素清 | The preparation method of coloured alumina dryer |
| CN1081393A (en) * | 1992-07-20 | 1994-02-02 | 中国科学院上海冶金研究所 | Highly effective drying agent and preparation method thereof |
| US20100248966A1 (en) * | 2005-01-07 | 2010-09-30 | Lynch James R | Homogeneous gas-evolving composition |
| CN107303482A (en) * | 2016-04-25 | 2017-10-31 | 蒋寿春 | A kind of chameleon fibre drier and its manufacture method and purposes |
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