CN103638824B - The preparation method of a kind of crosslinked inulin, fullerene composite membrane - Google Patents
The preparation method of a kind of crosslinked inulin, fullerene composite membrane Download PDFInfo
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- CN103638824B CN103638824B CN201310546111.8A CN201310546111A CN103638824B CN 103638824 B CN103638824 B CN 103638824B CN 201310546111 A CN201310546111 A CN 201310546111A CN 103638824 B CN103638824 B CN 103638824B
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- inulin
- fullerene
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- crosslinked
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- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229920001202 Inulin Polymers 0.000 title claims abstract description 34
- JYJIGFIDKWBXDU-MNNPPOADSA-N inulin Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)OC[C@]1(OC[C@]2(OC[C@]3(OC[C@]4(OC[C@]5(OC[C@]6(OC[C@]7(OC[C@]8(OC[C@]9(OC[C@]%10(OC[C@]%11(OC[C@]%12(OC[C@]%13(OC[C@]%14(OC[C@]%15(OC[C@]%16(OC[C@]%17(OC[C@]%18(OC[C@]%19(OC[C@]%20(OC[C@]%21(OC[C@]%22(OC[C@]%23(OC[C@]%24(OC[C@]%25(OC[C@]%26(OC[C@]%27(OC[C@]%28(OC[C@]%29(OC[C@]%30(OC[C@]%31(OC[C@]%32(OC[C@]%33(OC[C@]%34(OC[C@]%35(OC[C@]%36(O[C@@H]%37[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O%37)O)[C@H]([C@H](O)[C@@H](CO)O%36)O)[C@H]([C@H](O)[C@@H](CO)O%35)O)[C@H]([C@H](O)[C@@H](CO)O%34)O)[C@H]([C@H](O)[C@@H](CO)O%33)O)[C@H]([C@H](O)[C@@H](CO)O%32)O)[C@H]([C@H](O)[C@@H](CO)O%31)O)[C@H]([C@H](O)[C@@H](CO)O%30)O)[C@H]([C@H](O)[C@@H](CO)O%29)O)[C@H]([C@H](O)[C@@H](CO)O%28)O)[C@H]([C@H](O)[C@@H](CO)O%27)O)[C@H]([C@H](O)[C@@H](CO)O%26)O)[C@H]([C@H](O)[C@@H](CO)O%25)O)[C@H]([C@H](O)[C@@H](CO)O%24)O)[C@H]([C@H](O)[C@@H](CO)O%23)O)[C@H]([C@H](O)[C@@H](CO)O%22)O)[C@H]([C@H](O)[C@@H](CO)O%21)O)[C@H]([C@H](O)[C@@H](CO)O%20)O)[C@H]([C@H](O)[C@@H](CO)O%19)O)[C@H]([C@H](O)[C@@H](CO)O%18)O)[C@H]([C@H](O)[C@@H](CO)O%17)O)[C@H]([C@H](O)[C@@H](CO)O%16)O)[C@H]([C@H](O)[C@@H](CO)O%15)O)[C@H]([C@H](O)[C@@H](CO)O%14)O)[C@H]([C@H](O)[C@@H](CO)O%13)O)[C@H]([C@H](O)[C@@H](CO)O%12)O)[C@H]([C@H](O)[C@@H](CO)O%11)O)[C@H]([C@H](O)[C@@H](CO)O%10)O)[C@H]([C@H](O)[C@@H](CO)O9)O)[C@H]([C@H](O)[C@@H](CO)O8)O)[C@H]([C@H](O)[C@@H](CO)O7)O)[C@H]([C@H](O)[C@@H](CO)O6)O)[C@H]([C@H](O)[C@@H](CO)O5)O)[C@H]([C@H](O)[C@@H](CO)O4)O)[C@H]([C@H](O)[C@@H](CO)O3)O)[C@H]([C@H](O)[C@@H](CO)O2)O)[C@@H](O)[C@H](O)[C@@H](CO)O1 JYJIGFIDKWBXDU-MNNPPOADSA-N 0.000 title claims abstract description 34
- 229940029339 inulin Drugs 0.000 title claims abstract description 34
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 239000012528 membrane Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 229920000151 polyglycol Polymers 0.000 claims abstract description 6
- 239000010695 polyglycol Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000005213 imbibition Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 230000000873 masking effect Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 231100000749 chronicity Toxicity 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to the preparation method of a kind of crosslinked inulin, fullerene composite membrane, step is: (1) gets fullerene powder, crosses 200 mesh sieves after grinding; (2) get the inulin aqueous solution, add fullerene powder, carry out ultrasonic process, make fullerene powder and inulin aqueous solution evenly, add polyglycol solution, under microwave, react to obtain preparation liquid; (3) get preparation liquid to be filmed, the polyethylene glycol crosslinked inulin/fullerene composite membrane obtained has extraordinary water imbibition and larger specific area, is conducive to the absorption of composite membrane heavy metal.
Description
Technical field
The present invention relates to a kind of for the crosslinked inulin of adsorbing metal ions, the preparation method of fullerene composite membrane, belong to material processing field.
technical background
The survival and development of water to nature and the mankind plays irreplaceable effect, and along with the development of society, the heavy metal pollution of water body is more and more serious, and heavy metal pollution has the features such as disguise, chronicity and irreversibility.The biodegradation of metal ion non-differentiability, easily to accumulate in vivo.Because the waste water of industry-by-industry discharge is different, the complicated component of waste water, heavy metal ion wide variety, fluctuation of concentration is comparatively large, adds difficulty to wastewater treatment.
Summary of the invention
The object of this invention is to provide a kind of for the crosslinked inulin of adsorbing metal ions, the preparation method of fullerene composite membrane.
For realizing above object, the preparation method of crosslinked inulin of the present invention, fullerene composite membrane, step is:
(1) get fullerene powder, after grinding, cross 200 mesh sieves;
(2) the inulin aqueous solution that 100mL mass concentration is 4% is got, add fullerene powder, carry out ultrasonic process, make fullerene powder and inulin aqueous solution even, add the polyglycol solution that 3mL mass concentration is 1.4%, under microwave condition, 400r/min carries out stirring reaction, obtains preparation liquid;
(3) get preparation liquid to be filmed, the sodium hydroxide solution putting into 0.1mol/L after oven dry soaks takes off film, uses ethanol and distilled water repeatedly to rinse, until neutral, naturally dries, obtain polyethylene glycol crosslinked inulin/fullerene composite membrane.
Further, described fullerene is C60.
Further, the consumption of described C60 is 0.03-0.05g.
Further, described microwave power is 300-400W.
Further, described reaction temperature is 20-40 DEG C, and the reaction time is 5-15min.
The beneficial effect that the present invention produces is, the present invention is under microwave heating condition, by polyethylene glycol, inulin is cross-linked, carry out compound with fullerene again, the crosslinked inulin/fullerene composite membrane of generation has extraordinary water imbibition, and wet film hot strength and dry film hot strength all increase, wherein the particle diameter of fullerene is little, can better be distributed in film, increase specific area, be conducive to the absorption of composite membrane heavy metal.
Embodiment
Embodiment 1:
A kind ofly for the crosslinked inulin of adsorption of metal ions, the preparation method of fullerene composite membrane be:
(1) get fullerene powder, after grinding, cross 200 mesh sieves;
(2) get 100mL mass concentration be 4% the inulin aqueous solution put into solution, add 0.03g fullerene powder, carry out ultrasonic process, fullerene powder is mixed with solution, add the polyglycol solution that 3mL mass concentration is 1.4%, under microwave condition, 400r/min stirring reaction, microwave power is 300W, reaction temperature 20 DEG C, reaction time 10min, obtains preparation liquid;
(3) get preparation liquid masking, the sodium hydroxide solution putting into 0.1mol/L after oven dry soaks takes off film, uses ethanol and distilled water repeatedly to rinse, until neutral, naturally dries, obtain polyethylene glycol crosslinked inulin/fullerene composite membrane.
Crosslinked inulin obtained by the present embodiment, fullerene composite membrane, the saturated rear average moisture content that absorbs water is 427%, wet film hot strength 85.2MPa, dry film hot strength 107.3MPa, and specific area is 85.7m
2/ g.
Embodiment 2:
A kind ofly for the crosslinked inulin of adsorption of metal ions, the preparation method of fullerene composite membrane be:
(1) get fullerene powder, after grinding, cross 200 mesh sieves;
(2) get 100mL mass concentration be 4% the inulin aqueous solution put into solution, add 0.04g fullerene powder, carry out ultrasonic process, fullerene powder is mixed with solution, add the polyglycol solution that 3mL mass concentration is 1.4%, under microwave condition, 400r/min stirring reaction certain hour, microwave power is 350W, reaction temperature 30 DEG C, reaction time 5min, obtains preparation liquid;
(3) get preparation liquid masking, the sodium hydroxide solution putting into 0.1mol/L after oven dry soaks takes off film, uses ethanol and distilled water repeatedly to rinse, until neutral, naturally dries, obtain polyethylene glycol crosslinked inulin/fullerene composite membrane.
Crosslinked inulin obtained by the present embodiment, fullerene composite membrane, the saturated rear average moisture content that absorbs water is 446%, wet film hot strength 71.2MPa, dry film hot strength 99.8MPa, and specific area is 79.6m
2/ g.
Embodiment 3:
A kind ofly for the crosslinked inulin of adsorption of metal ions, the preparation method of fullerene composite membrane be:
(1) get fullerene powder, after grinding, cross 200 mesh sieves;
(2) get 100mL mass concentration be 4% the inulin aqueous solution put into solution, add 0.05g fullerene powder, carry out ultrasonic process, fullerene powder is mixed with solution, add the polyglycol solution that 3mL mass concentration is 1.4%, 400r/min stirring reaction certain hour under microwave condition,, microwave power is 400W, reaction temperature 40 DEG C, reaction time 10min, obtains preparation liquid;
(3) get preparation liquid masking, the sodium hydroxide solution putting into 0.1mol/L after oven dry soaks takes off film, uses ethanol and distilled water repeatedly to rinse, until neutral, naturally dries, obtain polyethylene glycol crosslinked inulin/fullerene composite membrane.
Crosslinked inulin obtained by the present embodiment, fullerene composite membrane, the saturated rear average moisture content that absorbs water is 410%, wet film hot strength 79.2MPa, dry film hot strength 99.9MPa, and specific area is 74.7m
2/ g.
Claims (5)
1. a preparation method for crosslinked inulin, fullerene composite membrane, is characterized in that: step is:
(1) get fullerene powder, after grinding, cross 200 mesh sieves;
(2) the inulin aqueous solution that 100mL mass concentration is 4% is got, add fullerene powder, carry out ultrasonic process, make fullerene powder and inulin aqueous solution even, add the polyglycol solution that 3mL mass concentration is 1.4%, under microwave condition, 400r/min carries out stirring reaction, obtains preparation liquid;
(3) get preparation liquid to be filmed, the sodium hydroxide solution putting into 0.1mol/L after oven dry soaks takes off film, uses ethanol and distilled water repeatedly to rinse, until neutral, naturally dries, obtain polyethylene glycol crosslinked inulin/fullerene composite membrane.
2. the preparation method of a kind of crosslinked inulin according to claim 1, fullerene composite membrane, is characterized in that: described fullerene is C60.
3. the preparation method of a kind of crosslinked inulin according to claim 2, fullerene composite membrane, is characterized in that: the consumption of described C60 is 0.03-0.05g.
4. the preparation method of a kind of crosslinked inulin according to claim 1, fullerene composite membrane, is characterized in that: described microwave power is 300-400W.
5. the preparation method of a kind of crosslinked inulin according to claim 1, fullerene composite membrane, it is characterized in that: described stirring reaction temperature is 20-40 DEG C, the reaction time is 5-15min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310546111.8A CN103638824B (en) | 2013-11-07 | 2013-11-07 | The preparation method of a kind of crosslinked inulin, fullerene composite membrane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310546111.8A CN103638824B (en) | 2013-11-07 | 2013-11-07 | The preparation method of a kind of crosslinked inulin, fullerene composite membrane |
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| Publication Number | Publication Date |
|---|---|
| CN103638824A CN103638824A (en) | 2014-03-19 |
| CN103638824B true CN103638824B (en) | 2015-11-18 |
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| CN105080366B (en) * | 2014-04-22 | 2017-05-31 | 中国石油化工股份有限公司 | A kind of reverse osmosis membrane and preparation method thereof |
| CN110339821A (en) * | 2019-08-08 | 2019-10-18 | 卫革 | A kind of method and apparatus preparing adsorbent for heavy metal using fullerene |
| CN115023819A (en) | 2019-11-27 | 2022-09-06 | 立方光伏股份有限公司 | Cross-linked surface coatings and interfacial layers for perovskite material photovoltaic devices |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001038175A (en) * | 1999-05-27 | 2001-02-13 | Toyobo Co Ltd | Composite semipermeable membrane |
| CN1424346A (en) * | 2002-12-20 | 2003-06-18 | 武汉大学 | Chitin mixed membrane containing Fullerene amine derivative and preparation thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030136727A1 (en) * | 1999-05-27 | 2003-07-24 | Hideki Yamada | Composite semipermeable membrane |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001038175A (en) * | 1999-05-27 | 2001-02-13 | Toyobo Co Ltd | Composite semipermeable membrane |
| CN1424346A (en) * | 2002-12-20 | 2003-06-18 | 武汉大学 | Chitin mixed membrane containing Fullerene amine derivative and preparation thereof |
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| CN103638824A (en) | 2014-03-19 |
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Inventor after: Cai Minli Inventor before: Su Jianli |
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Effective date of registration: 20170524 Address after: 515041, Xinjin building, No. 89, Songshan Road, Longhu District, Guangdong, Shantou Patentee after: Guangdong able new material technology Co., Ltd. Address before: 266061 Shandong, Laoshan, Hongkong East Road, No. Pioneering Park, biological park, room 248, No. 239 Patentee before: Qingdao Wenchuang Science & Technology Co., Ltd. |
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Address after: 515000 Guangdong city of Shantou province (Free Trade Zone) after a processing zone Guang'ao Jiang 522A room five layer Patentee after: Guangdong able new material technology Co., Ltd. Address before: 515041, Xinjin building, No. 89, Songshan Road, Longhu District, Guangdong, Shantou Patentee before: Guangdong able new material technology Co., Ltd. |
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