CN104383794A - Chemical drying agent and preparation method thereof - Google Patents
Chemical drying agent and preparation method thereof Download PDFInfo
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- CN104383794A CN104383794A CN201410668135.5A CN201410668135A CN104383794A CN 104383794 A CN104383794 A CN 104383794A CN 201410668135 A CN201410668135 A CN 201410668135A CN 104383794 A CN104383794 A CN 104383794A
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Abstract
The invention discloses a chemical drying agent and a preparation method thereof. The preparation method of the chemical drying agent comprises the step of firstly preparing a graphene foam material, dissolving calcium chloride in water to obtain a calcium chloride aqueous solution, submerging the graphene foam material in the calcium chloride aqueous solution, and finally drying the graphene foam material containing the calcium chloride aqueous solution to obtain the chemical drying agent. The chemical drying agent prepared by the method has good moisture absorption performance; the scattering of the drying agent caused by breakage of a drying agent package bag is avoided; the chemical drying agent and the preparation method thereof can be applied to fields of drying and storing foods.
Description
Technical field
The present invention relates to drier field, especially a kind of chemical drier and preparation method thereof.
Background technology
The management and control of moisture and the yield of product are closely bound up, and with food, under suitable temperature and humidity, the bacterium in food and mould just can breed with surprising rapidity, make food spoilage, cause and make moist and look change.Drier can remove the moisture in moist material, and it is often divided into two classes: chemical drier, as calcium sulfate and calcium chloride etc., generates hydrate carry out drying by being combined with water; Physical dryness agent, as silica gel and activated alumina etc., carries out drying by physical absorption water.Drier is in the market coated in gas permeability bag mainly with graininess or pulverous form, but such bag breaks because of quality problems or by colliding sometimes, causes graininess or Powdered drier to be scattered, and pollutes required dry article or product.For food, if be mixed into drier and eaten by mistake, likely cause human injury or poisoning.
Summary of the invention
In view of the defect that prior art exists, the invention provides a kind of preparation method of chemical drier, in order to improve the defect that desiccant particle of the prior art or powder are easily scattered.
Another object of the present invention is to provide a kind of chemical drier of non-corrosive, reusable, high adsorption capacity.
The preparation method of a kind of chemical drier provided by the invention, comprise the following steps: first prepare grapheme foam material, then by calcium chloride with water-soluble solution, again grapheme foam material is dipped in above-mentioned solution, finally the grapheme foam material containing above-mentioned calcium chloride water is given drying, i.e. obtained chemical drier sheet.The dissolving step of described calcium chloride preferably first heats water to 25-50 DEG C, then adds calcium chloride and is configured to calcium chloride supersaturated solution.Be dipped in by grapheme foam material in the step of above-mentioned solution, the volume of calcium chloride solution did not at least have grapheme foam material, and dip time is preferably 2h-24h.
The preparation method of described grapheme foam material is: 1) in the aqueous solution of graphene oxide, add surfactant, then alkaline solution adjust ph is added to form the mixed solution that pH value is 8-12, described mixed solution is poured in hydrothermal reaction kettle, be warming up to 120 DEG C-240 DEG C and be incubated 6-48h, obtaining the wet gel block that graphene sheet layer overlaps mutually; 2) wet gel block in step 1 is carried out freezing oven dry, obtain grapheme foam material.The step of described freezing oven dry is preferably: first control freezing drying chamber and carry out precooling within the scope of temperature is-50 to-60 DEG C, precooling duration can determine according to the volume of wet gel block, to ensure the complete crystallization of moisture in described wet gel block; Then open vavuum pump, carry out vacuum and drain.The ratio of quality and the number of copies of described graphene oxide and described surfactant is preferably 99:1-99:3.The concentration of described graphene oxide is preferably 0.5mg/mL-5mg/mL.Described surfactant is preferably nonionic surface active agent.
The present invention also provides a kind of chemical drier, adopts the preparation method of above-mentioned chemical drier to obtain.
Beneficial effect: drier prepared by the present invention, make use of that Graphene specific area is large, porous and be the characteristic of solid-state structure, calcium chloride is attached in grapheme foam material, the hygroscopicity of calcium chloride can be given full play to, and the three-dimensional macro structure of grapheme foam material, make calcium chloride no longer powdered, even if packaging bag is broken, do not worry the leakage of calcium chloride drier, the drying of the article such as food can be applied to yet.
Accompanying drawing illustrates:
The Graphene wet gel block of Fig. 1 obtained by the embodiment of the present invention 1;
The SEM figure of the grapheme foam material of Fig. 2 obtained by the embodiment of the present invention 1.
The SEM figure of the grapheme foam material of Fig. 3 obtained by the embodiment of the present invention 9.
Detailed description of the invention
Following examples are the preferred embodiment of the present invention, do not limit protection scope of the present invention with this.Therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Embodiment 1:
The polyvinylpyrrolidone getting 97 mass parts graphene oxides and 3 mass parts puts into water, ultrasonic disperse in ultrasonic cell disrupte machine, and ultrasonic power is 100W, and the mass concentration being mixed with graphene oxide is the mixed aqueous solution of 2mg/mL, then adds NH
3h
2o regulates the pH value of above-mentioned mixed aqueous solution to be 10.4, then puts into water heating kettle, is warming up to 180 DEG C and is incubated 12h, obtains the wet gel block that graphene sheet layer overlaps mutually, as shown in Figure 1.Freezing 24h at wet gel block is put into-56 DEG C, opens vavuum pump after the complete crystallization of the crystallization water in wet gel block, carries out vacuum and drains, obtain grapheme foam material.Get this grapheme foam material to observe under a scanning electron microscope, as shown in Figure 2, this graphene sheet layer overlaps mutually, forms more hole.
At 50 DEG C, prepare the saturated calcium chloride solution of 100mL, then above-mentioned grapheme foam material is immersed 2h in described saturated calcium chloride solution, pull oven dry out, be i.e. obtained chemical drier.
Described drier is at room temperature put into the environment that relative humidity is 90%, and surveying its wettability after 30 days is 285%.Then the chemical drier after moisture absorption is put into baking oven to dry, then put into the environment that relative humidity is 90%, surveying its wettability after 30 days is 255%.
Embodiment 2:
The ratio of quality and the number of copies of controlled oxidization Graphene and polyvinylpyrrolidone is respectively 99:1,95:5,93:7,90:10, keeps other reaction conditions identical with embodiment 1, to prepare grapheme foam material.Wherein, when the ratio of quality and the number of copies of graphene oxide and polypyrrole alkane ketone is 90:10, the wet gel fragmentation prepared after hydro-thermal is caved in, and does not thus carry out subsequent experimental.And other ratios of quality and the number of copies can obtain more complete wet gel block.
The grapheme foam material obtained by different quality portion rate to be immersed at 50 DEG C 2h in the saturated calcium chloride solution of 100mL of preparation, takes out and dries, and obtains three kinds of different chemical driers.
Above-mentioned three kinds of different drier are at room temperature put into the environment that relative humidity is 90%, after 30 days, surveys its wettability, as shown in the table.
Chemical drier wettability obtained under different quality portion rate compares
| Ratio of quality and the number of copies | 99:1 | 97:3 | 95:5 | 93:7 |
| Wettability | 233％ | 285％ | 198％ | 96％ |
Embodiment 3
The concentration of controlled oxidization Graphene is respectively 0.1mg/mL, 0.5mg/mL, 1.0mg/mL, 3mg/mL, 5mg/mL, keeps reaction condition identical with embodiment 1, to prepare grapheme foam material.Wherein, the graphene oxide of 0.1mg/mL is too low due to concentration, self assembly can not go out Graphene wet gel block, therefore not do subsequent experimental.
The grapheme foam material that different graphene oxide concentration obtains to be immersed at 50 DEG C 2h in the saturated calcium chloride solution of 100mL of preparation, to take out and dry, obtain four kinds of different chemical driers.
Above-mentioned three kinds of different drier are at room temperature put into the environment that relative humidity is 90%, after 30 days, surveys its wettability, as shown in the table.
Chemical drier wettability obtained under variable concentrations compares
| Concentration | 0.5 | 1.0 | 2 | 3 | 5 |
| Wettability | 176％ | 223％ | 285％ | 290％ | 198 |
Embodiment 4
The pH value of controlled oxidization Graphene and polypyrrole alkane ketone is 8.2 and 11.7, keeps other conditions identical with embodiment 1, and obtained chemical drier at room temperature relative humidity is leave standstill 30 days in the environment of 90%, records its wettability and is respectively 93% and 137%.
Embodiment 5
Control hydrothermal temperature and be respectively 120 DEG C and 240 DEG C, keep other conditions identical with embodiment 1, obtained chemical drier at room temperature relative humidity is leave standstill 30 days in the environment of 90%, records its wettability and is respectively 76% and 210%.
Embodiment 6
The control hydro-thermal reaction time is respectively 3h, 6h, 24h, 48h, keeps other conditions identical with embodiment 1, to prepare grapheme foam material.Wherein, the hydro-thermal time of 3h is too short, can not obtain Graphene wet gel block, therefore not do subsequent experimental.
The grapheme foam material that the different hydro-thermal time obtains to be immersed at 50 DEG C 2h in the saturated calcium chloride solution of 100mL of preparation, to take out and dry, obtain four kinds of different chemical driers.
Above-mentioned four kinds of different chemical driers are at room temperature put into the environment that relative humidity is 90%, after 30 days, surveys its wettability, as shown in the table.
Under the different hydro-thermal time, obtained chemical drier wettability compares
| The hydro-thermal time | 6 | 12 | 24 | 48 |
| Wettability | 183％ | 285％ | 265％ | 255％ |
Embodiment 7
At room temperature prepare the saturated calcium chloride solution of 100mL, then grapheme foam material obtained for embodiment 1 is immersed 2h in described saturated calcium chloride solution, pull oven dry out, be i.e. obtained chemical drier.Described chemical drier at room temperature relative humidity is leave standstill 30 days in the environment of 90%, and recording its wettability is 186%.
Embodiment 8
At room temperature prepare the saturated calcium chloride solution of 100mL, 48h in saturated calcium chloride solution shown in then being immersed by grapheme foam material obtained for embodiment 1, pulls oven dry out, i.e. obtained chemical drier.Described chemical drier at room temperature relative humidity is leave standstill 30 days in the environment of 90%, records its wettability and is respectively 190%.
Embodiment 9
Change the polyvinylpyrrolidone of 3 mass parts in embodiment 1 into polyethylene glycol, control other reaction conditions identical with embodiment 1, to prepare grapheme foam material.Get this grapheme foam material to observe under an electron microscope, as shown in Figure 3, this grapheme foam material has certain network structure.
Described grapheme foam material is immersed in 2h in the saturated calcium chloride solution of 100mL of preparation at 50 DEG C, takes out and dry, obtain chemical drier.Described chemical drier is at room temperature put into the environment that relative humidity is 90%, and surveying its wettability after 30 days is 67%.
Claims (9)
1. the preparation method of a chemical drier, comprise the following steps: first prepare grapheme foam material, then by calcium chloride with water-soluble solution, again grapheme foam material is dipped in above-mentioned solution, finally the grapheme foam material containing above-mentioned calcium chloride water is given drying, i.e. obtained chemical drier sheet.
2. the preparation method of chemical drier according to claim 1, is characterized in that: the dissolving step of described calcium chloride, for first to heat water to 25-50 DEG C, then adds calcium chloride and is configured to calcium chloride supersaturated solution.
3. the preparation method of chemical drier according to claim 1, is characterized in that: be describedly dipped in by grapheme foam material in the step of above-mentioned solution, and the volume of calcium chloride solution did not at least have grapheme foam material, and dip time is 2h-24h.
4. the preparation method of chemical drier according to claim 1, it is characterized in that: the preparation method of described grapheme foam material is: 1) in the aqueous solution of graphene oxide, add surfactant, then alkaline solution adjust ph is added to form the mixed solution that pH value is 8-12, described mixed solution is poured in hydrothermal reaction kettle, be warming up to 120 DEG C-240 DEG C and be incubated 6-48h, obtaining the wet gel block that graphene sheet layer overlaps mutually; 2) wet gel block in step 1 is carried out freezing oven dry, obtain grapheme foam material.
5. the preparation method of chemical drier according to claim 4, it is characterized in that: the step of described freezing oven dry is: first control freezing drying chamber and carry out precooling within the scope of temperature is-50 to-60 DEG C, precooling duration can determine according to the volume of wet gel block, to ensure the complete crystallization of moisture in described wet gel block; Then open vavuum pump, carry out vacuum and drain.
6. the preparation method of chemical drier according to claim 4, is characterized in that: the ratio of quality and the number of copies of described graphene oxide and described surfactant is 99:1-99:3.
7. the preparation method of chemical drier according to claim 4, is characterized in that: the concentration of described graphene oxide is 0.5mg/mL-5mg/mL.
8. the preparation method of chemical drier according to claim 4, is characterized in that: described surfactant is nonionic surface active agent.
9. a chemical drier, is characterized in that: adopt the preparation method of the chemical drier described in claim 1-9 any one to obtain.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694915A (en) * | 2015-11-25 | 2016-06-22 | 北京旭碳新材料科技有限公司 | Composition for flame-retardant composite material and graphene flame-retardant foam and preparation method and application of foam |
| CN105994374A (en) * | 2016-05-21 | 2016-10-12 | 杨勇 | Antibacterial mildewproof agent |
| WO2017201096A1 (en) * | 2016-05-16 | 2017-11-23 | Nitto Denko Corporation | Graphene oxide moisture adsorbing device |
| CN111009864A (en) * | 2019-12-06 | 2020-04-14 | 广东华创电器设备有限公司 | Bus duct connection cover plate graphene heat dissipation device |
| CN112537768A (en) * | 2019-09-23 | 2021-03-23 | 中国科学院上海硅酸盐研究所苏州研究院 | High-strength three-dimensional graphene macroscopic body and preparation method thereof |
| CN113215828A (en) * | 2021-06-10 | 2021-08-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Perforated graphene aerogel moisture absorption fiber, and preparation method and application thereof |
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| CN102600802A (en) * | 2012-03-16 | 2012-07-25 | 华中师范大学 | Graphite-base carbon dioxide adsorbent and preparation method thereof |
| US20130161847A1 (en) * | 2011-12-27 | 2013-06-27 | Gi Byoung HWANG | Apparatus and method for fabricating antimicrobial hybrid materials of natural product and carbon nanomaterials |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694915A (en) * | 2015-11-25 | 2016-06-22 | 北京旭碳新材料科技有限公司 | Composition for flame-retardant composite material and graphene flame-retardant foam and preparation method and application of foam |
| WO2017201096A1 (en) * | 2016-05-16 | 2017-11-23 | Nitto Denko Corporation | Graphene oxide moisture adsorbing device |
| CN105994374A (en) * | 2016-05-21 | 2016-10-12 | 杨勇 | Antibacterial mildewproof agent |
| CN112537768A (en) * | 2019-09-23 | 2021-03-23 | 中国科学院上海硅酸盐研究所苏州研究院 | High-strength three-dimensional graphene macroscopic body and preparation method thereof |
| CN112537768B (en) * | 2019-09-23 | 2023-09-08 | 中国科学院上海硅酸盐研究所苏州研究院 | High-strength three-dimensional graphene macroscopic body and preparation method thereof |
| CN111009864A (en) * | 2019-12-06 | 2020-04-14 | 广东华创电器设备有限公司 | Bus duct connection cover plate graphene heat dissipation device |
| CN113215828A (en) * | 2021-06-10 | 2021-08-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Perforated graphene aerogel moisture absorption fiber, and preparation method and application thereof |
| CN113215828B (en) * | 2021-06-10 | 2022-11-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Perforated graphene aerogel moisture absorption fiber, and preparation method and application thereof |
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| CN104383794B (en) | 2016-03-30 |
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Effective date of registration: 20191211 Address after: Room 207, main office building, No.118 Longxing Road, Haining Economic Development Zone, Haining City, Jiaxing City, Zhejiang Province Patentee after: Haining Economic Development Industrial Park Development and Construction Co., Ltd Address before: 523000, Dongguan, Guangdong, Dongcheng District Province, main road, Dongcheng, South Road, No. 81, brilliant business building, 8 floor, A03 one Patentee before: Dongguan City Guanxin Enterprise Management Consulting Co., Ltd. |
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