CN102690534B - Preparation method of novel surface grafting modification inorganic nano humidity controlling material - Google Patents
Preparation method of novel surface grafting modification inorganic nano humidity controlling material Download PDFInfo
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- CN102690534B CN102690534B CN2012101183246A CN201210118324A CN102690534B CN 102690534 B CN102690534 B CN 102690534B CN 2012101183246 A CN2012101183246 A CN 2012101183246A CN 201210118324 A CN201210118324 A CN 201210118324A CN 102690534 B CN102690534 B CN 102690534B
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Abstract
The invention discloses a preparation method of a novel surface grafting modification inorganic nano humidity controlling material, comprising the steps of: A) preparing purified nanotube halloysite; B) preparing acidized nanotube halloysite; C) preparing organic modified nanotube halloysite; and D) adding the organic modified nanotube halloysite into an ethanol aqueous solution and further adding benzoyl peroxide and a hydrophilic monomer into the ethanol aqueous solution, wherein the ethanol aqueous solution is composed of one part of ethanol and 50-300 parts of water, the ratio of the organic modified nanotube halloysite to the ethanol aqueous solution is 1:10-30, the amount of the benzoyl peroxide is 0.2-3% of the amount of the organic modified nanotube halloysite, the hydrophilic monomer is acrylic acid or acrylamide whose amount is 50-300% of the amount of the organic modified nanotube halloysite; and stirring the mixture for 2-3 hours at a temperature ranged from 50 DEG C to 80 DEG C, filtering, and drying to acquire the novel surface grafting modification inorganic nano humidity controlling material. The surface grafting modification inorganic nano humidity controlling material of the invention is characterized by high humidity response speed.
Description
Technical field
The invention belongs to the preparing technical field of modified inorganic material, especially relate to a kind of preparation method of novel surface graft modification inorganic nano humidity adjusting material,
Background technology
Atmospheric moisture is the important environmental parameters that and people's life and production have substantial connection.Humidity is all significant to the protection of human comfort, IAQ (indoor air quality), article.The control of temperature at present is fairly simple effective, but still more difficult to the control of atmospheric moisture, and especially concerning historical relic, medicine, high-grade jewelry etc., the infringement that the damage ratio temperature that the ambient relative humidity fluctuation causes causes is large.Therefore humidity is control effectively and seems even more important and urgent.Humidity adjusting material is to need not the Nonrenewable energy resources such as power consumption, have the good ecological environment material nd of adjusting air humidity ability automatically, to save energy, improve amenity, promote that the Sustainable development etc. of ecotope is significant.
The nanotube halloysite is a kind of aluminium silicate mineral, has the hollow nano tubular structure, and caliber is between 10～30nm, and pipe range is between 10～30um, and surface and interlayer contain active hydroxyl.Its chemical constitution is identical with kaolinite, but than kaolinite, contains higher moisture, has specific surface area larger, the feature of good heat stability.It is with a wide range of applications at aspects such as catalyzer, functional materials, stupalith, nano composite material, environment protection, but, as synthesis of molecular sieve on chemical industry and the carrier of making catalyzer, is used as filler etc. in plastics, rubber and paint industry.In fact, the special nanotubes structure that the nanotube halloysite has and surface thereof and interlayer exist the structural performance of active hydroxyl to provide theoretical basis for it has humidity, and this structural performance is conducive to the further improvement of its moisture-absorbing/releasing.
The hydrophilic macromolecule that has certain polymerization degree on nanotube halloysite surface grafting, on the one hand its wet volume capacity is improved, be beneficial on the other hand the nanotube halloysite further compound with other organic humidity controlling material, the organic/inorganic composite humidity adjusting material that processability is more excellent.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of novel surface graft modification inorganic nano humidity adjusting material.For this reason, the technical solution used in the present invention is such:
A) powdery nanotube halloysite (200-500 order) is added to the water with weight ratio 1: 10～100, centrifugation 10～30min, filter the halloysite that suspends in ore pulp, and drying, make the purified nanotubes halloysite;
B) the nanotube halloysite after purifying is joined mass percent concentration in 3～10% hydrochloric acid soln take weight ratio 1: 10～20, at 20～30 ℃ of temperature, stirred 2～3 hours, drying, make acidifying nanotube halloysite;
C) the nanotube halloysite of getting after acidifying joins in the ethanolic soln of mass percent concentration 5～10% with weight ratio 1: 5～15, ultrasonic wave is disperseed 10～30min, the silane coupling agent KH-590 solution that adds pure halloysite amount 2～8% (mass percent), ultrasonic wave is disperseed 40～60min, filter and drying, make organic modified nano pipe halloysite;
D) organic modified nano pipe halloysite is joined in the aqueous solution of ethanol, add therein again benzoyl peroxide and hydrophilic monomer, wherein the ratio of aqueous ethanolic solution is 1 part of ethanol, 50～300 parts, water, and the ratio of organic modified nano pipe halloysite and aqueous ethanolic solution is 1: 10～30; The consumption of benzoyl peroxide is 0.2～3% of organic modified nano pipe halloysite; Hydrophilic monomer is vinylformic acid or acrylamide, and its consumption is 50～300% of organic modified nano pipe halloysite; Under 50～80 ℃, stirred 2～3 hours after mixing, filter and drying, make novel surface graft modification inorganic nano humidity adjusting material.
The surface graft modification inorganic nano humidity adjusting material of the present invention's preparation, characteristics with humidity fast response time, simultaneously due to the hydrophilic macromolecule that has certain polymerization degree on nanotube halloysite surface grafting, on the one hand its wet volume capacity is improved, be beneficial on the other hand the nanotube halloysite further compound with other organic humidity controlling material, the organic/inorganic composite humidity adjusting material that processability is better.
Embodiment
A) powdery nanotube halloysite is sieved for twice with 200 orders and 500 orders, get particle diameter at 200-500 purpose powdery nanotube halloysite, take 1kg, join in 50kg water, centrifugation 30min, filter the halloysite that suspends in ore pulp, drying, make the purified nanotubes halloysite;
B) the nanotube halloysite 700g after purifying being joined the 10kg mass percent concentration is in 10% hydrochloric acid soln, at 20～30 ℃ of temperature, to stir 2 hours, and drying, make acidifying nanotube halloysite;
C) get nanotube halloysite 700g after acidifying, join in the ethanolic soln of 10L mass percent concentration 5%, ultrasonic wave is disperseed 20min, add 400g silane coupling agent KH-590 solution, ultrasonic wave is disperseed 40～60min, filters and drying, makes organic modified nano pipe halloysite;
D) get organic modified nano pipe halloysite 500g and join in the ethanolic soln of 10L mass percent concentration 2%, then add therein benzoyl peroxide 5g and acrylamide 400g; Under 50～80 ℃, stirred 2～3 hours after mixing, filter and drying, make novel surface graft modification inorganic nano humidity adjusting material.
Claims (1)
1. the preparation method of a novel surface graft modification inorganic nano humidity adjusting material is characterized in that adopting following steps:
A) be that 200-500 purpose powdery nanotube halloysite is added to the water with weight ratio 1: 10～100 with the order number, centrifugation 10～30min, filter the halloysite that suspends in ore pulp, and drying, make the purified nanotubes halloysite;
B) the nanotube halloysite after purifying is joined mass percent concentration in 3～10% hydrochloric acid soln take weight ratio 1: 10～20, at 20～30 ℃ of temperature, stirred 2～3 hours, drying, make acidifying nanotube halloysite;
C) the nanotube halloysite of getting after acidifying joins in the ethanolic soln of mass percent concentration 5～10% with weight ratio 1: 5～15, ultrasonic wave is disperseed 10～30min, the silane coupling agent KH-590 solution that adds pure halloysite amount 2～8% (mass percent), ultrasonic wave is disperseed 40～60min, filter and drying, make organic modified nano pipe halloysite;
D) organic modified nano pipe halloysite is joined in the aqueous solution of ethanol, add therein again benzoyl peroxide and hydrophilic monomer, wherein the ratio of aqueous ethanolic solution is 1 part of ethanol, 50～300 parts, water, and the ratio of organic modified nano pipe halloysite and aqueous ethanolic solution is 1: 10～30; The consumption of benzoyl peroxide is 0.2～3% of organic modified nano pipe halloysite; Hydrophilic monomer is acrylamide, and its consumption is 50～300% of organic modified nano pipe halloysite; Under 50～80 ℃, stirred 2～3 hours after mixing, filter and drying, make novel surface graft modification inorganic nano humidity adjusting material.
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| CN102690534B true CN102690534B (en) | 2013-11-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3530622A4 (en) * | 2016-10-24 | 2019-11-06 | JFE Mineral Company, Ltd. | Halloysite powder and method for producing halloysite powder |
Families Citing this family (7)
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| CN104119704B (en) * | 2013-04-27 | 2016-05-11 | 中国科学院化学研究所 | The surface modifying treatment of halloysite nanotubes |
| CN103290725B (en) * | 2013-06-01 | 2015-07-08 | 浙江理工大学 | Method for preparing organic/inorganic nano composite surface sizing agent |
| CN103627219B (en) * | 2013-10-25 | 2015-04-22 | 浙江理工大学 | Organic modification method of Halloysite nanotubes |
| CN104874357A (en) * | 2015-05-04 | 2015-09-02 | 河南师范大学 | Preparation method of modified halloysite oil absorbent |
| CN110726757B (en) * | 2019-10-17 | 2021-12-03 | 电子科技大学 | Humidity sensor based on halloysite nanotube and preparation method thereof |
| CN111482160A (en) * | 2020-04-30 | 2020-08-04 | 杭州亨玛电力科技有限公司 | Humidity regulating tablet and preparation method thereof |
| CN112248598B (en) * | 2020-11-02 | 2021-04-13 | 安徽火峰电气有限公司 | Anti-condensation humidity regulating tablet |
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