CN1850937A - High temperature-resistant polymer phase-transition material - Google Patents
High temperature-resistant polymer phase-transition material Download PDFInfo
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- CN1850937A CN1850937A CN 200510066697 CN200510066697A CN1850937A CN 1850937 A CN1850937 A CN 1850937A CN 200510066697 CN200510066697 CN 200510066697 CN 200510066697 A CN200510066697 A CN 200510066697A CN 1850937 A CN1850937 A CN 1850937A
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- transition material
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Abstract
The invention relates to a high temperature resistance macromolecule phase change material-polyether fatty acid ester. The main chain of the polyether is polyethylene glycol or polytetramethylene glycol and the fatty acid acyl is stearic acid acyl, palmitic acid acyl or lauric acid acyl.
Description
Technical field
The invention relates to a kind of phase change macromolecular material, and particularly relevant for a kind of resistant to elevated temperatures phase change macromolecular material.
Background technology
Phase-transition material is a kind ofly can be changed to liquid phase or be changed to the material of solid phase by liquid phase by solid phase in specific range of temperatures, and can follow absorption or the release of a large amount of latent heat (latent heat) when changing.Common phase-transition material is paraffin wax hydrocarbons (paraffinic hydrocarbons; C
nH
2n+2).The maximum characteristics of phase-transition material are when its absorption or when discharging a large amount of latent heat, can allow the temperature maintenance of system certain.Therefore one of its common application is and utilizes this heat preservation property to make the insulation textiles.
At present, the mode that phase-transition material is integrated into fabric has two kinds.First kind for being coated on the surface of textile fibres or fabric after being embedded in phase-transition material in the microcapsule; Second kind then be embedded in phase-transition material in the microcapsule after, be added to again in the spinning solution of acryl, make the acryl fiber with wet type spin processes (wet spinning) again.Above-mentioned dual mode, all be that phase-transition material is made into microcapsule, first kind of mode wherein is to utilize back arrangement processing mode, allows the microcapsule that are embedded with phase-transition material attached to textile fibres or fabric face, because of coming off easily, so its application has certain restriction.The second way because use solvent, has the problem in solvent recuperation and the environmental protection for directly using in spinning.
Yet, general common regenerated fiber, as acryl fiber (acrylic fibers), nylon fiber (nylonfibers), trevira (polyester fibers), polypropylene fibre (polypropylene fibers) and other similar artificial fibers or the like, have only the acryl fiber can use the wet type spin processes to make, other most regenerated fibers all are to utilize melt-spinning (melt spinning) method to make.Since melt spinning method carry out temperature up to 200-380 ℃, and every square of inch must bear the pressure up to 3000 pounds.So concerning at present common phase-transition material, as the alkanes of long carbochain and the carboxylic ester compound (carboxylic ester) that U.S. Patent Publication No. is disclosed for No. 2004/0026659, because thermogravimetric analysis shows that the maximum thermogravimetric loss temperature of above-mentioned materials is about 150 ℃, therefore under the condition of melt-spinning, may allow the phase-transition material branch take off.At present more existing researchs are underway, to address the above problem.
For example, in No. 6689466 patent of the U.S. " Stable phase change materials for usein temperature regulating synthetic fibers; fabrics and textiles ", disclose a kind of stable phase transformation composition and comprise phase-transition material, antioxidant and thermo-stabilizer.Wherein, above-mentioned antioxidant and thermo-stabilizer are responsible for providing the oxidation-resistance and the thermostability of phase-transition material, can add in the melting master batch to allow this phase change form, to carry out various high molecular melt-processed.
In No. 6793856 patent of the U.S. " Melt spinable concentrate pellets havingenhanced reversible thermal properties ", announcement allows phase-transition material be coated in the microcapsule, or allows it directly be concentrated in the melt-spinning master batch.Wherein, the principal constituent of melt-spinning master batch is thermal plastic high polymer (thermoplastic polymer).
In TaiWan, China No. 587110 patent " many composition fiber and manufacture method with reversible thermal property of reinforcement " relevant, disclose multi-constituent fibre (multi-component fiber) by the melt spinning method manufacturing with above-mentioned two pieces of patents.The conjugated fibre that this multi-constituent fibre is made up of at least two kinds of fibers is as sea island fiber, core-sheath-type fiber etc.
Summary of the invention
The purpose of this invention is to provide a kind of resistant to elevated temperatures phase-transition material, make it be suitable for high temperature process.
Another object of the present invention provides a kind of have low melting point and high boiling phase-transition material, makes it be suitable for being applied on the adjusting human body temperature.
According to above-mentioned and other purposes of the present invention, a kind of high temperature-resistant polymer phase-transition material is proposed, it is to be a kind of polyether fatty acid ester, its soliqueous phase change temperature range is 0-80 ℃, and maximum thermogravimetric loss temperature is greater than 350 ℃.
According to a preferred embodiment of the present invention, the polyether backbone of above-mentioned polyether fatty acid ester partly is preferably polyoxyethylene glycol or polytetramethylene glycol, preferable 200 gram/ears to 20 not that are about of the molecular weight of polyoxyethylene glycol wherein, 000 gram/ear not, the molecular weight of polytetramethylene glycol is preferable to be about the ear to 3 of 650 grams/not, the ear of 000 gram/not.The carbon number of the fatty acid acyl of above-mentioned polyether fatty acid ester two end portions is preferably 4 to 28, is more preferred from stearic acid acyl group, palmitinic acid acyl group or lauric acid acyl group.
According to above-mentioned and other purposes of the present invention, the manufacture method of above-mentioned polyether fatty acid ester is proposed.Above-mentioned polyether fatty acid ester is to be carried out esterification and got by polyether glycol and lipid acid, or is carried out esterification and got by polyether glycol and lipid acid acyl chlorides.
Allow above-mentioned polyether fatty acid ester carry out thermogravimetric analysis, show that the maximum thermogravimetric loss temperature of above-mentioned materials is about 370-400 ℃, be enough to carry out melt-spinning processing.And the fusing point of above-mentioned polyether fatty acid ester is close with body temperature about about 16.3-57.6 ℃, therefore very suitablely is used for regulating body temperature.In addition, the raw material of above-mentioned polyether fatty acid ester is very easy to be obtained, and therefore can significantly reduce production costs.
Embodiment
The invention provides a kind of high temperature-resistant polymer phase change material with low melting point and high boiling point characteristic.Because people's shell temperature is about about 30-35 ℃, if the fusing point of phase change material then can be applicable on the clothing of regulate body temperature near people's the body temperature.With the regenerated fiber of melt-spinning manufacturing, required processing temperature is many about 200-380 ℃, therefore need have high boiling phase change material, is beneficial to make regenerated fiber with melt-spinning again.
Phase change material provided by the present invention is a kind of polyether fatty acid ester, and its soliqueous phase change temperature range is 0-80 ℃, and maximum thermogravimetric loss temperature is greater than 350 ℃.The polyether backbone of above-mentioned polyether fatty acid ester partly is preferably polyoxyethylene glycol (polyethylene glycol; PEG) or polytetramethylene glycol (polytetramethylene glycol; PTMG); Preferable 200 gram/ears to 20 not that are about of the molecular weight of polyoxyethylene glycol wherein, the ear of 000 gram/not, the molecular weight of polytetramethylene glycol is preferable to be about the ear to 3 of 650 grams/not, the ear of 000 gram/not.The carbon number of the fatty acid acyl of above-mentioned polyether fatty acid ester two end portions is preferably 4 to 28, for example stearic acid acyl group (stearoyl group; 18 carbon), palmitinic acid acyl group (palmitoyl group; 16 carbon) or lauric acid acyl group (lauroyl group; 12 carbon).
Above-mentioned polyether fatty acid ester can utilize polyether glycol and carry out esterification with lipid acid and get, or is carried out esterification and got by polyether glycol and fatty acid acyl halogen (for example lipid acid acyl chlorides, lipid acid acylbromide or lipid acid acyl iodides).Above-mentioned polyether glycol is preferably polyoxyethylene glycol or polytetramethylene glycol; Preferable 200 gram/ears to 20 not that are about of the molecular weight of polyoxyethylene glycol wherein, the ear of 000 gram/not, the molecular weight of polytetramethylene glycol is preferable to be about the ear to 3 of 650 grams/not, the ear of 000 gram/not.
Above-mentioned lipid acid can be saturated fatty acid and derivative thereof, or has the unsaturated fatty acids and the derivative thereof of a carbon-carbon double bond.The carbonatoms of lipid acid is preferably 4 to 28, for example stearic acid, palmitinic acid or lauric acid.Above-mentioned fatty acid acyl halogen can be saturated fatty acid carboxylic acid halides element and derivative thereof, or has the unsaturated fatty acids carboxylic acid halides element and the derivative thereof of a carbon-carbon double bond.The carbonatoms of fatty acid acyl halogen is preferably 4 to 28, for example stearic acid acyl chlorides, palmitic acid chloride or lauric acid acyl chlorides.
According to above-mentioned, it is as follows with the manufacture method that above-mentioned polyether fatty acid ester is described to list several embodiment.
Embodiment one
The Polyethylene Glycol-600 of 60 grams, stearic acid, 1 milliliter sulfuric acid and 200 milliliters the toluene of 57 grams are mixed, carry out reflux (reflux) reaction and reduce the moisture content of reactive system the inside, in order to the carrying out of esterification.Behind product purification, promptly get Polyethylene Glycol-600-SUNSOFT Q-182S.Then, use hot differential scanning instrument (Differential Scanning Calorimetry; DSC) measure the fusing point of Polyethylene Glycol-600-SUNSOFT Q-182S, recording fusing point is 38.4 ℃, with thermogravimetric analyzer (ThermalGravity Analyzer; TGA) thermogravimetric of analyzing Polyethylene Glycol-600-SUNSOFT Q-182S is lost curve, records its maximum thermogravimetric loss temperature and is about 389 ℃.
Embodiment two
After right-toluenesulphonic acidss that the stearic acid and 1.0 of the polyethylene glycol 1500s of 150 grams, 57 grams are restrained mix, above-mentioned mixture is heated and vacuumizes, in order to the moisture content of removing in the reactive system.Behind purifying, promptly get polyethylene glycol 1500-SUNSOFT Q-182S.Fusing point by the measured polyethylene glycol 1500-SUNSOFT Q-182S of hot differential scanning instrument is about 35.0 ℃, loses temperature with the maximum thermogravimetric of the measured polyethylene glycol 1500-SUNSOFT Q-182S of thermogravimetric analyzer and is about 392 ℃.
Embodiment three
With the stearic acid acyl chlorides of 200 polytetramethylene glycols that restrain, 2000,60.6 grams and 200 milliliters N, dinethylformamide (N, N-dimethylformamide; DMF) mix, carry out reacting by heating then, and catch the hydrochloric acid gas that also neutralization reaction generated simultaneously.Behind purifying, promptly get polytetramethylene glycol 2000-SUNSOFT Q-182S.Fusing point by the measured polytetramethylene glycol 2000-SUNSOFT Q-182S of hot differential scanning instrument is about 28.9 ℃, loses temperature with the maximum thermogravimetric of the measured polytetramethylene glycol 2000-SUNSOFT Q-182S of thermogravimetric analyzer and is about 398 ℃.
List the rerum natura of the prepared polymeric phase change material that goes out below.Listed in Table 1 is the fusing point and the maximum thermogravimetric loss temperature of cithrol, lists the fusing point and the maximum thermogravimetric loss temperature of polytetramethylene glycol fatty acid ester in table two.Table one demonstrates and uses polyoxyethylene glycol institute synthetic polyether fatty acid ester, and its melting range is about about 32-58 ℃, and maximum thermogravimetric loss temperature is about 387-395 ℃, therefore very is suitable for being applied to make regenerated fiber with melt-spinning.Table two also demonstrates and uses polytetramethylene glycol institute synthetic polyether fatty acid ester, and its fusing point is lower slightly, be about about 16-34 ℃ and, maximum thermogravimetric loss temperature is about about 376-396 ℃.
Table one: the fusing point of cithrol and maximum thermogravimetric loss temperature
| Polyether fatty acid ester | Fusing point (℃) | Maximum thermogravimetric loss temperature (℃) |
| Polyethylene glycol 6000-SUNSOFT Q-182S | 57.6 | 394 |
| Polyethylene glycol 6000-dilaurate | 57.6 | 389 |
| Macrogol 4000-SUNSOFT Q-182S | 55.0 | 390 |
| Macrogol 4000-dilaurate | 54.4 | - |
| Macrogol 2000-SUNSOFT Q-182S | 49.5 | 389 |
| Polyethylene glycol 1500-SUNSOFT Q-182S | 44.8 | 393 |
| Cetomacrogol 1000-SUNSOFT Q-182S | 38.3 | - |
| Polyethylene Glycol-600-SUNSOFT Q-182S | 38.5 | 389 |
| Poly(oxyethylene glycol) 400-SUNSOFT Q-182S | 45.9 | 387 |
| Macrogol 200-SUNSOFT Q-182S | 45.0 | 388 |
Table two: the fusing point of polytetramethylene glycol fatty acid ester and maximum thermogravimetric loss temperature
| Polyether fatty acid ester | Fusing point (℃) | Maximum thermogravimetric loss temperature (℃) |
| Polytetramethylene glycol 3000-SUNSOFT Q-182S | 29.0 | - |
| Polytetramethylene glycol 2000-SUNSOFT Q-182S | 28.9 | 399 |
| Polytetramethylene glycol 2000-dilaurate | 26.4 | 391 |
| Polytetramethylene glycol 1800-SUNSOFT Q-182S | 29.6 | - |
| Polytetramethylene glycol 1800-dilaurate | 24.3 | - |
| Polytetramethylene glycol 1000-SUNSOFT Q-182S | 31.0 | - |
| Polytetramethylene glycol 850-SUNSOFT Q-182S | 33.4 | 376 |
| Polytetramethylene glycol 850-dipalmitate | 29.3 | - |
| Polytetramethylene glycol 850-dilaurate | 16.3 | - |
By the invention described above preferred embodiment as can be known, the present invention utilizes handy industrial raw material to synthesize to have low melting point and resistant to elevated temperatures new phase change material.Therefore, very be suitable for carrying out melt-spinning, can regulate the textiles of human body temperature to make with the regenerated fiber raw material.Polymeric phase change material provided by the present invention, its application mode can be phase change material is mixed in the melt-spun master batch, re-use melt spinning method and make core-sheath-type fiber or sea island fiber.Also phase change material can be dissolved in the spinning solution, use the wet type spin processes to make regenerated fiber.Also can be with after the phase change material fusion, again with spray pattern by in its infiltrated fiber structure, make fiber construct have temperature regulation and heat storing and heat preserving function.So high temperature resistant being widely used property of phase change material provided by the present invention.
Though the present invention discloses as above with preferred embodiment; yet it is not in order to limit the present invention; any person skilled in the art person; without departing from the spirit and scope of the present invention; when the change that can do various equivalences or replacement, so protection scope of the present invention is when looking accompanying being as the criterion that the application's claim scope defined.
Claims (16)
1. high temperature-resistant polymer phase-transition material, this polymer phase-transition material is a polyether fatty acid ester, its soliqueous phase change temperature range is 0-80 ℃, and maximum thermogravimetric loss temperature is greater than 350 ℃.
2. high temperature-resistant polymer phase-transition material as claimed in claim 1 is characterized in that the polyether backbone of this polyether fatty acid ester partly is polyoxyethylene glycol or polytetramethylene glycol.
3. high temperature-resistant polymer phase-transition material as claimed in claim 2, the molecular weight that it is characterized in that this polyoxyethylene glycol are about the ear to 20 of 200 grams/not, the ear of 000 gram/not.
4. high temperature-resistant polymer phase-transition material as claimed in claim 2, the molecular weight that it is characterized in that this polytetramethylene glycol are 650 gram/ears to 3 not, the ear of 000 gram/not.
5. high temperature-resistant polymer phase-transition material as claimed in claim 1, the carbon number that it is characterized in that the fatty acid acyl of this polyether fatty acid ester two end portions is 4 to 28.
6. high temperature-resistant polymer phase-transition material as claimed in claim 1, the fatty acid acyl that it is characterized in that this polyether fatty acid ester two end portions are stearic acid acyl group, palmitinic acid acyl group or lauric acid acyl group.
7. the manufacture method of a high temperature-resistant polymer phase-transition material, it is to be carried out esterification and got by a polyether glycol and a lipid acid, or carry out esterification and get by this polyether glycol and a fatty acid acyl halogen, wherein this fatty acid acyl halogen is lipid acid acyl chlorides, lipid acid acylbromide or lipid acid acyl iodides.
8. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this polyether glycol is polyoxyethylene glycol or polytetramethylene glycol.
9. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 8, the molecular weight that it is characterized in that this polyoxyethylene glycol are the ears to 20 of 200 grams/not, the ear of 000 gram/not.
10. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 8, the molecular weight that it is characterized in that this polytetramethylene glycol are the ears to 3 of 650 grams/not, the ear of 000 gram/not.
11. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this lipid acid is saturated fatty acid and derivative thereof, its carbonatoms is 4 to 28.
12. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this lipid acid is unsaturated fatty acids and the derivative thereof with a carbon-carbon double bond, its carbonatoms is 4 to 28.
13. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this lipid acid is stearic acid, palmitinic acid or lauric acid.
14. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this fatty acid acyl halogen is saturated fatty acid carboxylic acid halides element and derivative thereof, its carbonatoms is 4 to 28.
15. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this fatty acid acyl halogen is unsaturated fatty acids carboxylic acid halides element and the derivative thereof with a carbon-carbon double bond, its carbonatoms is 4 to 28.
16. the manufacture method of high temperature-resistant polymer phase-transition material as claimed in claim 7 is characterized in that this fatty acid acyl halogen is stearic acid carboxylic acid halides element, palmitinic acid carboxylic acid halides element or lauric acid carboxylic acid halides element.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002342A (en) * | 2010-09-26 | 2011-04-06 | 大连工业大学 | Method for preparing waste acrylic fiber and fatty acid combined phase change material |
| CN102533225A (en) * | 2012-01-05 | 2012-07-04 | 新疆太阳能科技开发公司 | Formula of solar season-span heat-storage composite heat-accumulation material |
| CN113684554A (en) * | 2020-05-19 | 2021-11-23 | 财团法人纺织产业综合研究所 | Temperature-regulating nylon fiber |
| CN113929838A (en) * | 2021-11-18 | 2022-01-14 | 西南石油大学 | Preparation of high-salt-resistant self-elasticizing type hydrophobically associating polymer and application of polymer in fracturing fluid |
-
2005
- 2005-04-22 CN CN 200510066697 patent/CN1850937A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002342A (en) * | 2010-09-26 | 2011-04-06 | 大连工业大学 | Method for preparing waste acrylic fiber and fatty acid combined phase change material |
| CN102002342B (en) * | 2010-09-26 | 2013-05-08 | 大连工业大学 | Method for preparing waste acrylic fiber and fatty acid combined phase change material |
| CN102533225A (en) * | 2012-01-05 | 2012-07-04 | 新疆太阳能科技开发公司 | Formula of solar season-span heat-storage composite heat-accumulation material |
| CN102533225B (en) * | 2012-01-05 | 2013-12-11 | 新疆太阳能科技开发公司 | Solar season-span heat-storage composite heat-accumulation material |
| CN113684554A (en) * | 2020-05-19 | 2021-11-23 | 财团法人纺织产业综合研究所 | Temperature-regulating nylon fiber |
| CN113929838A (en) * | 2021-11-18 | 2022-01-14 | 西南石油大学 | Preparation of high-salt-resistant self-elasticizing type hydrophobically associating polymer and application of polymer in fracturing fluid |
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