CN106554754A - The preparation method of polyethylene glycol/nano silicon composite phase-change material - Google Patents
The preparation method of polyethylene glycol/nano silicon composite phase-change material Download PDFInfo
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- CN106554754A CN106554754A CN201510632486.5A CN201510632486A CN106554754A CN 106554754 A CN106554754 A CN 106554754A CN 201510632486 A CN201510632486 A CN 201510632486A CN 106554754 A CN106554754 A CN 106554754A
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Abstract
The invention provides a kind of preparation method of polyethylene glycol/nano silicon composite phase-change material.First polyethylene glycol is reacted with silane coupler and generates the performed polymer with siloxanes key end group, after then be well mixed prepolymer with tetraethyl orthosilicate, then by acid-catalyzed hydrolysis-condensation reaction, prepare PEG-SiO2Sol system, obtains gel by the volatilization of solvent, is drying to obtain polyethylene glycol/nano silicon composite phase-change material.Polyethylene glycol/nano silicon composite phase-change material prepared by the present invention can significantly lift the thermal conductivity of compound system, and enthalpy of phase change and phase transition temperature are substantially reduced.
Description
Technical field
The present invention relates to the preparation field of organic chemistry composite phase-change material, and in particular to a kind of polyethylene glycol/receive
The preparation method of rice silica composite phase-change material.
Background technology
Once there is the report prepared to composite phase-change material in the past, the new technology of comparison is exactly polyethylene glycol/hard charcoal
The preparation of black grafting composite phase-change material, the primary grade of white carbon is nanoscale, but be long placed in, be modified and
Necessarily occur to reunite after compound, in compound system, particle diameter reaches hundreds of nanometers, belongs to micron scale construction, and
And the hydroxyl value on its surface is limited, the maximum percent grafting of polyethylene glycol is caused to be subject to certain restrictions.
The content of the invention
2 points of problems for more than, the invention provides a kind of polyethylene glycol/nano silicon composite phase-change material
The preparation method of material, prepares the composite phase-change material with higher percent grafting.First by polyethylene glycol and silane
Coupling agent reaction generates the performed polymer with siloxanes key end group, then mixes prepolymer with tetraethyl orthosilicate
After even, then by acid-catalyzed hydrolysis-condensation reaction, PEG-SiO is prepared2Sol system, by the volatilization of solvent
Gel is obtained, polyethylene glycol/nano silicon composite phase-change material is drying to obtain.
Concrete preparation method includes following two steps：
1) prepared by the PEG performed polymers of siloxanes terminal：5～10gPEG being vacuum dried is added to into taper
In bottle, 15～25mL toluene is added in conical flask, 1.5～2.0g KH-560 is instilled, is stirred, then
The BFEE of 0.1～0.2g is instilled again, in 70～90 DEG C of oil bath pans, 3.5～4.5h of stirring reaction, so
Afterwards the solution for obtaining is filtered with filter paper, the boron hydroxide white sedimentation generated after removing boron trifluoride hydrolysis
Particle, obtains final product the toluene solution of the polyethylene glycol of siloxanes terminal.
2) sol-gel process prepares polyethylene glycol/nano silicon composite phase-change material：To step 1) it is obtained
Toluene solution in add 3.5～4.5g TEOS, after stirring, ultrasound 5～8 minutes, in ultrasonic procedure
Hydrochloric acid/the ethanol/water solution of PH=1 is added dropwise over, with the addition of aqueous hydrochloric acid solution, system gradually becomes breast
White, forms water-in-oil emulsion system, ultrasonic emulsification 5～8 minutes afterwards, by the emulsion for obtaining as
In 40～50 DEG C of oil bath pans, 10～15h of stirring reaction obtains sol system；It is subsequently poured into the training of diameter 25cm
In foster ware, it is aged 3～5 days under natural environment, obtains gel rubber system, culture dish is positioned over into vacuum drying oven then
In 110 DEG C be vacuum dried 2 days, obtain final product polyethylene glycol/nano silicon composite phase-change material.
Wherein, the molecular weight of polyethylene glycol is 800；
Step 1) described in 3.5～4.5h of stirring reaction, step 2) described in 10～15h of stirring reaction, use
Agitating mode be magnetic agitation；
Step 2) described in the hydrochloric acid/ethanol/water solution for being added dropwise over pH=1, the addition of water is institute in system
There is 1 times of siloxanes key mole, the consumption of ethanol is 5～8mL.
Beneficial effect
Polyethylene glycol/nano silicon composite phase-change material prepared by the present invention can significantly lift complex
The thermal conductivity of system, enthalpy of phase change and phase transition temperature are substantially reduced.
Specific embodiment
Test material and test apparatus：
Polyethylene glycol：Molecular weight 800, Chemical Reagent Co., Ltd., Sinopharm Group；
KH-560：Analysis is pure, and Guangzhou Supreme Being is into trade Co., Ltd；
Tetraethyl orthosilicate (TEOS)：With SiO2Content meter >=28.0%, Tianjin great Mao chemical reagent factories；
Hydrochloric acid：Analyze pure, the mass fraction 36.0～38.0% of hydrochloric acid, Guangzhou Yun Hui trade Co., Ltds；
BFEE：Boron trifluoride content 46.8～47.8%, Yang Yuan Chemical Co., Ltd.s of Changshu City；
Ultrasonic cell disruption instrument：Model 5-450D, Branson companies of the U.S.；
Electronic balance：Model JJ200, Shuan Jie testers factory of Changshu City；
PLM with heating stage：Model BXS 1-P/LINKAMTHMS600, Guangzhou southeast Kechuang science and technology
Co., Ltd；
Embodiment 1
1) prepared by the PEG performed polymers of siloxanes terminal：The 8gPEG being vacuum dried is added to into conical flask
In, 20mL toluene is added in conical flask, 1.65g KH-560 is instilled, is stirred, then instill again
The BFEE of 0.1g, in 90 DEG C of oil bath pans, then the solution for obtaining filtered by stirring reaction 4h
Paper is filtered, the boron hydroxide white sedimented particle generated after removing boron trifluoride hydrolysis, obtains final product siloxanes end
The toluene solution of the polyethylene glycol at end.
2) sol-gel process prepares polyethylene glycol/nano silicon composite phase-change material：To step 1) it is obtained
Toluene solution in add 4g TEOS, after stirring, ultrasound 5 minutes, in ultrasonic procedure dropwise plus
Enter the hydrochloric acid/ethanol/water solution of PH=1, with the addition of aqueous hydrochloric acid solution, system gradually becomes milky,
Form water-in-oil emulsion system, ultrasonic emulsification 5 minutes afterwards, by the emulsion for obtaining as 50 DEG C of oil bath pans
Interior, stirring reaction 12h obtains sol system；It is subsequently poured in the culture dish of diameter 25cm, natural environment
Lower ageing 5 days, obtains gel rubber system, and culture dish is positioned over 110 DEG C of vacuum drying 2 in vacuum drying oven then
My god, obtain final product polyethylene glycol/nano silicon composite phase-change material.
Jing is tested, and the phase transition temperature of composite phase-change material is 23.5 DEG C, and enthalpy of phase change is 87.2J/g, and thermal conductivity is
0.299W/ (mK), the thermal conductivity than pure PEG-800 increased 23.29%.
Above example can illustrate, polyethylene glycol/nano silicon composite phase-change material prepared by the present invention
The thermal conductivity of compound system can be significantly lifted, enthalpy of phase change and phase transition temperature are substantially reduced.
Claims (4)
1. the preparation method of a kind of polyethylene glycol/nano silicon composite phase-change material, it is characterised in that：It is first
First polyethylene glycol is reacted with silane coupler and generates the performed polymer with siloxanes key end group, then by prepolymer
After being well mixed with tetraethyl orthosilicate, then by acid-catalyzed hydrolysis-condensation reaction, PEG-SiO is prepared2Sol
System, obtains gel by the volatilization of solvent, is drying to obtain polyethylene glycol/nano silicon composite phase-change material；
Concrete preparation method includes following two steps：
1) prepared by the PEG performed polymers of siloxanes terminal：5～10gPEG being vacuum dried is added to into taper
In bottle, 15～25mL toluene is added in conical flask, 1.5～2.0g KH-560 is instilled, is stirred, then
The BFEE of 0.1～0.2g is instilled again, in 70～90 DEG C of oil bath pans, 3.5～4.5h of stirring reaction, so
Afterwards the solution for obtaining is filtered with filter paper, the boron hydroxide white sedimentation generated after removing boron trifluoride hydrolysis
Particle, obtains final product the toluene solution of the polyethylene glycol of siloxanes terminal；
2) sol-gel process prepares polyethylene glycol/nano silicon composite phase-change material：To step 1) it is obtained
Toluene solution in add 3.5～4.5g TEOS, after stirring, ultrasound 5～8 minutes, in ultrasonic procedure
Hydrochloric acid/the ethanol/water solution of PH=1 is added dropwise over, with the addition of aqueous hydrochloric acid solution, system gradually becomes breast
White, forms water-in-oil emulsion system, ultrasonic emulsification 5～8 minutes afterwards, by the emulsion for obtaining as
In 40～50 DEG C of oil bath pans, 10～15h of stirring reaction obtains sol system；It is subsequently poured into the training of diameter 25cm
In foster ware, it is aged 3～5 days under natural environment, obtains gel rubber system, culture dish is positioned over into vacuum drying oven then
In 110 DEG C be vacuum dried 2 days, obtain final product polyethylene glycol/nano silicon composite phase-change material.
2. according to a kind of preparation of polyethylene glycol/nano silicon composite phase-change material described in claim 1
Method, it is characterised in that：The molecular weight of described polyethylene glycol is 800.
3. according to a kind of preparation of polyethylene glycol/nano silicon composite phase-change material described in claim 1
Method, it is characterised in that：Step 1) described in 3.5～4.5h of stirring reaction, step 2) described in stirring it is anti-
10～15h is answered, the agitating mode used is magnetic agitation.
4. according to a kind of preparation of polyethylene glycol/nano silicon composite phase-change material described in claim 1
Method, it is characterised in that：Step 2) described in the hydrochloric acid/ethanol/water solution for being added dropwise over pH=1, water plus
Enter amount for 1 times of all siloxanes key moles in system, the consumption of ethanol is 5～8mL.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867467A (en) * | 2017-04-14 | 2017-06-20 | 青岛大学 | The method and phase-change material of polyethylene glycol phase-change material performance are improved using modified silica |
| CN110041891A (en) * | 2019-05-21 | 2019-07-23 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide phase change materials |
| CN110105925A (en) * | 2019-05-21 | 2019-08-09 | 温州大学 | Cetylamine/silicon dioxide composite shape-stabilized phase phase-change material preparation method |
| CN110157315A (en) * | 2019-05-23 | 2019-08-23 | 南京珈时新材料科技有限公司 | A kind of insulating moulding coating and its application containing hollow silica microsphere |
| CN111647161A (en) * | 2020-05-15 | 2020-09-11 | 江门市金信恒科技有限公司 | Organic silicon resin and preparation method and application thereof |
| CN114106810A (en) * | 2021-11-05 | 2022-03-01 | 中国地质大学（北京） | Nano silicon dioxide, nano composite slickwater fracturing fluid, preparation method and application |
| US20240018404A1 (en) * | 2022-07-13 | 2024-01-18 | King Fahd University Of Petroleum And Minerals | Doped phase change material and method of preparation thereof |
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2015
- 2015-09-29 CN CN201510632486.5A patent/CN106554754A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867467A (en) * | 2017-04-14 | 2017-06-20 | 青岛大学 | The method and phase-change material of polyethylene glycol phase-change material performance are improved using modified silica |
| CN106867467B (en) * | 2017-04-14 | 2022-06-03 | 青岛大学 | Method for improving performance of polyethylene glycol phase-change material by using modified silicon dioxide and phase-change material |
| CN110041891A (en) * | 2019-05-21 | 2019-07-23 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide phase change materials |
| CN110105925A (en) * | 2019-05-21 | 2019-08-09 | 温州大学 | Cetylamine/silicon dioxide composite shape-stabilized phase phase-change material preparation method |
| CN110041891B (en) * | 2019-05-21 | 2020-10-30 | 温州大学 | Preparation method of polyethylene glycol/silicon dioxide shaped phase change material |
| CN110105925B (en) * | 2019-05-21 | 2020-11-13 | 温州大学 | Preparation method of hexadecylamine/silicon dioxide composite shape-stabilized phase change material |
| CN110157315A (en) * | 2019-05-23 | 2019-08-23 | 南京珈时新材料科技有限公司 | A kind of insulating moulding coating and its application containing hollow silica microsphere |
| CN110157315B (en) * | 2019-05-23 | 2021-06-04 | 南京特粒材料科技有限公司 | Heat insulation coating containing hollow silica microspheres and application thereof |
| CN111647161A (en) * | 2020-05-15 | 2020-09-11 | 江门市金信恒科技有限公司 | Organic silicon resin and preparation method and application thereof |
| CN114106810A (en) * | 2021-11-05 | 2022-03-01 | 中国地质大学（北京） | Nano silicon dioxide, nano composite slickwater fracturing fluid, preparation method and application |
| CN114106810B (en) * | 2021-11-05 | 2023-01-03 | 中国地质大学（北京） | Nano silicon dioxide, nano composite slickwater fracturing fluid, preparation method and application |
| US20240018404A1 (en) * | 2022-07-13 | 2024-01-18 | King Fahd University Of Petroleum And Minerals | Doped phase change material and method of preparation thereof |
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