CN103691411B - A kind of formaldehyde adsorbent containing shitosan and beta-schardinger dextrin-and preparation method thereof - Google Patents
A kind of formaldehyde adsorbent containing shitosan and beta-schardinger dextrin-and preparation method thereof Download PDFInfo
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- CN103691411B CN103691411B CN201410012978.XA CN201410012978A CN103691411B CN 103691411 B CN103691411 B CN 103691411B CN 201410012978 A CN201410012978 A CN 201410012978A CN 103691411 B CN103691411 B CN 103691411B
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- shitosan
- beta
- schardinger dextrin
- formaldehyde
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000003463 adsorbent Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 229920000858 Cyclodextrin Polymers 0.000 abstract description 7
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 4
- 239000002250 absorbent Substances 0.000 abstract description 3
- 230000002745 absorbent Effects 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229930040373 Paraformaldehyde Natural products 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 229920002866 paraformaldehyde Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of formaldehyde adsorbent containing shitosan and beta-schardinger dextrin-and preparation method thereof.Formaldehyde adsorbent is made up of shitosan and beta-schardinger dextrin-, and shitosan and beta-schardinger dextrin-mass ratio are 1:4 ~ 1:8.Preparation method comprises: be dissolved in by shitosan in hydrochloric acid; Mix with beta-schardinger dextrin-solution again, stir; Slow dropping glutaraldehyde solution is in mixed liquor, and heating is uniformly mixed liquid under inert gas shielding; In reactant liquor, add sodium hydroxide solution makes product separate out, and filters, washes with water and wash with acetone to neutrality; Vacuum drying.Formaldehyde adsorbent of the present invention combines recognition performance and the shitosan adsorption function of cyclodextrin, absorption property is good, stable in properties, favorable reproducibility, selective good, greatly can reduce the content of formaldehyde gas in space, and absorbent preparation technique is simple, cost is low, pollution-free, be applicable to suitability for industrialized production.
Description
Technical field
The invention belongs to sorbing material Synthesis and applications field, specifically, relate to a kind of formaldehyde adsorbent and preparation method thereof.
Background technology
Formaldehyde, also known as formaldehyde, has intense stimulus smell, is the healthy indoor air pollutants of a kind of important harm people.Along with the progress of society, the raising of living standard, people are also improving constantly the requirement of environment, and increasing people starts to pay close attention to indoor environmental quality.Research formaldehyde in indoor air purification techniques, improves IAQ, has very important significance.
The method removed for formaldehyde in air at present has absorption method, catalytic oxidation, biological degradation method, plasma technique etc.These methods respectively have pluses and minuses, and wherein the most frequently used be absorption method.Only stronger suction-operated is had to material that is nonpolar or low pole at present based on the solid absorbent of all kinds of active carbon and goods thereof, and very little to the formaldehyde absorbing capacity of strong polarity, and easily discharged by secondary when absorption is saturated and temperature is higher.Therefore, need a kind of low cost of exploitation badly, to human body without harm, the scavenging material of the Formaldehyde Pollution of Indoor Air that aldehydes removal efficiency is higher.
Shitosan is the de-acetyl product of chitin, strand has abundant amino and hydroxyl two kinds of reactive groups, can interact with the aldehyde radical of formaldehyde, for the indoor free formaldehyde of adsorption removal.CN101327424A discloses one shitosan, the Powdered formaldehyde adsorbent that manganese dioxide and active carbon Homogeneous phase mixing obtain.Beta-schardinger dextrin-(β-CD) has the special molecular structure of " interior hydrophobic, outer hydrophilic " and multiple chiral molecules, can be used as " host " envelope difference " object " compound, forms the inclusion complex that structure is special.Based on this special construction, β-CD has the performance of selective absorption pollutant in the air that particularly humidity is larger from air.In addition, cyclodextrin also has excellent deodorizing effect.By immobilized for cyclodextrin on shitosan, not only combine recognition performance and the shitosan absorption property of cyclodextrin, the stability of all right reinforcing material and absorption property.At present, there is no the relevant report that the immobilized β of shitosan-CD is used as solid-phase gas pollutant absorbent.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of and contain formaldehyde adsorbent of shitosan and beta-schardinger dextrin-and preparation method thereof.
For achieving the above object, the present invention adopts following technical scheme:
A kind of formaldehyde adsorbent, be made up of shitosan and beta-schardinger dextrin-, shitosan and beta-schardinger dextrin-mass ratio are 1:4 ~ 1:8.
The preparation method of above-mentioned formaldehyde adsorbent, comprises the steps:
Step one, shitosan to be dissolved in hydrochloric acid solution, then with beta-schardinger dextrin-solution by volume 1:1 mix, stirred at ambient temperature;
In mixed liquor in step 2, the mixed solution that obtains in step one: the ratio of glutaraldehyde solution volume ratio 10:1 ~ 50:1, drip glutaraldehyde solution with the speed of 0.1 ~ 1.0mL/min, and at inert gas shielding and 50 ~ 80 DEG C, stir 1 ~ 24 hour;
Adding sodium hydroxide solution in step 3, the mixed solution that obtains in step 2 makes product separate out, and filters and washes product with water to neutral, then with acetone washing, at 60 DEG C, vacuum drying is stablized to product quality;
Step 4, pulverized by the solid product obtained, be sieved into the adsorbent of variable grain size in step 3, sealing saves backup.
In above-mentioned preparation method, the concentration of hydrochloric acid solution described in step one is 0.05 ~ 0.5mol/L, and the mass fraction of glutaraldehyde solution described in step 2 is 15% ~ 25%.
In above-mentioned preparation method, the concentration of sodium hydroxide solution described in step 3 is 0.5 ~ 3mol/L, is 1:3 ~ 1:8 with the volume ratio of mixed liquor.
Compared with prior art, the present invention has following beneficial effect:
The formaldehyde adsorbent of the immobilized beta-schardinger dextrin-of shitosan provided by the present invention, it combines recognition performance and the shitosan adsorption function of cyclodextrin, stable in properties, favorable reproducibility, selective good, greatly can reduce the content of formaldehyde gas in space, be applicable to the absorption of trace toxic, etchant gas in the air such as PARA FORMALDEHYDE PRILLS(91,95) in the indoor or automobile such as office, bedroom, parlor, hotel.Its adsorbent cost is low, and preparation technology is simple, pollution-free, is applicable to suitability for industrialized production.
Detailed description of the invention
Embodiment 1: the preparation of the immobilized beta-schardinger dextrin-adsorbent of shitosan:
Step one, 4g shitosan is dissolved in 200mL concentration is in the hydrochloric acid of 0.1mol/L, and adds the cyclodextrin solution that 200mL contains 24g beta-schardinger dextrin-;
Step 2, the mixed liquor obtained in step one is stirred 1h at 25 DEG C after, dripping 24mL concentration with the speed of 0.8mL/min is the glutaraldehyde solution of 25%;
Step 3, by the mixed liquor that obtains in step 2 at nitrogen protection and 70 DEG C, stop reaction after stirring 6h;
Step 4, be that the sodium hydroxide solution of 1mol/L joins in the mixed liquor obtained in step 3 product is separated out by 70mL concentration, filter, wash with water with acetone washing to neutrality, finally at 60 DEG C, vacuum drying is stablized to product quality;
Step 5, the solid product obtained in step 4 is sieved into the adsorbent that granular size is 0.20 ~ 0.45mm, sealing saves backup.
Embodiment 2: the preparation of the immobilized beta-schardinger dextrin-adsorbent of shitosan:
Step one, 4g shitosan is dissolved in 150mL concentration is in the hydrochloric acid of 0.2mol/L, and adds the cyclodextrin solution that 150mL contains 16g beta-schardinger dextrin-;
Step 2, the mixed liquor obtained in step one is stirred 1h at 25 DEG C after, dripping 30mL concentration with the speed of 1mL/min is the glutaraldehyde solution of 20%;
Step 3, by the mixed liquor that obtains in step 2 at nitrogen protection and 70 DEG C, stop reaction after stirring 6h;
Step 4, be that the sodium hydroxide solution of 1mol/L joins in the mixed liquor obtained in step 3 product is separated out by 70mL concentration, filter, wash with water with acetone washing to neutrality, finally at 60 DEG C, vacuum drying is stablized to product quality;
Step 5, the solid product obtained in step 4 is sieved into the adsorbent that granular size is 0.20 ~ 0.45mm, sealing saves backup.
Embodiment 3: the absorption property of the adsorbent PARA FORMALDEHYDE PRILLS(91,95) of embodiment 1
By dynamic experiment method, investigate the absorption property of adsorbent PARA FORMALDEHYDE PRILLS(91,95).At ambient temperature, get 0.5g and put into by the adsorbent that embodiment 1 is made the adsorption column that internal diameter is 7mm, using air as carrier gas, pass into formaldehyde by Bubbling method to adsorbent bed.Be 1000h in air speed
-1, air inlet concentration of formaldehyde is 46mg/m
3time, the equilibrium adsorption capacity of formaldehyde is 13mg (formaldehyde)/g (adsorbent).Adsorb saturated after, at 60 DEG C, the air directly passing into 100mL/min carries out purging desorption, and formaldehyde desorption rate is greater than 98%, completes once absorption/de-adsorption cycle.After three circulations, the adsorbance of formaldehyde is 12mg (formaldehyde)/g (adsorbent), illustrates that the immobilized beta-schardinger dextrin-adsorbent of shitosan can be recycled.
Embodiment 4: the absorption property of the adsorbent PARA FORMALDEHYDE PRILLS(91,95) of embodiment 2
Experimental technique is identical with embodiment 3, adsorbent is changed into adsorbent prepared by embodiment 2, and the equilibrium adsorption capacity of formaldehyde is 11mg (formaldehyde)/g (adsorbent).Adsorb saturated after, at 60 DEG C, the air directly passing into 100mL/min carries out purging desorption, and formaldehyde desorption rate is greater than 98%, completes once absorption/de-adsorption cycle.After three circulations, the adsorbance of formaldehyde is 10.2mg (formaldehyde)/g (adsorbent), illustrates that the immobilized beta-schardinger dextrin-adsorbent of shitosan can be recycled.
Claims (1)
1. a formaldehyde adsorbent, it is characterized in that being made up of shitosan and beta-schardinger dextrin-, shitosan and beta-schardinger dextrin-mass ratio are 1:4 ~ 1:8; Preparation method comprises the steps:
Step one, shitosan to be dissolved in hydrochloric acid solution, then with beta-schardinger dextrin-solution by volume 1:1 mix, stirred at ambient temperature;
In mixed liquor in step 2, the mixed solution that obtains in step one: the ratio of glutaraldehyde solution volume ratio 10:1 ~ 50:1, drip glutaraldehyde solution with the speed of 0.1 ~ 1.0mL/min, and at inert gas shielding and 50 ~ 80 DEG C, stir 1 ~ 24 hour;
Adding sodium hydroxide solution in step 3, the mixed solution that obtains in step 2 makes product separate out, and filters and washes product with water to neutral, then with acetone washing, at 60 DEG C, vacuum drying is stablized to product quality;
Step 4, pulverized by the solid product obtained, be sieved into the adsorbent of variable grain size in step 3, sealing saves backup;
The concentration of hydrochloric acid solution described in step one is 0.05 ~ 0.5mol/L, and the mass fraction of glutaraldehyde solution described in step 2 is 15% ~ 25%;
The concentration of sodium hydroxide solution described in step 3 is 0.5 ~ 3mol/L, is 1:3 ~ 1:8 with the volume ratio of mixed liquor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI483773B (en) * | 2014-04-09 | 2015-05-11 | Prior Company Ltd | Aqueous formaldehyde scavenger composition |
| CN104028237A (en) * | 2014-06-07 | 2014-09-10 | 中山大学惠州研究院 | Chitosan immobilized beta-cyclodextrin formaldehyde absorbent with fragrance release function |
| CN105776961A (en) * | 2016-02-18 | 2016-07-20 | 吉林省珍贝壳环保新材料有限公司 | Comprehensive environment-friendly shell powder coating |
| CN106189613A (en) * | 2016-07-19 | 2016-12-07 | 同济大学 | A kind of indoor air purification environmental protection coating material for timber buildings and preparation method thereof |
| CN109161359A (en) * | 2018-08-01 | 2019-01-08 | 福州市晋安区绿奇鑫环保科技有限公司 | It is a kind of with the environment Protection composite floor board and preparation method thereof for going formaldehyde function |
| CN108930199A (en) * | 2018-08-01 | 2018-12-04 | 福州市晋安区绿奇鑫环保科技有限公司 | It is a kind of with the wallpaper and preparation method thereof for going formaldehyde function |
| CN113786506A (en) * | 2021-10-21 | 2021-12-14 | 青岛科技大学 | Composition for removing old people smell and preparation and application of preparation thereof |
| CN114208848B (en) * | 2022-01-20 | 2023-02-28 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods thereof |
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| CN1490349A (en) * | 2002-10-15 | 2004-04-21 | 浙江大学 | Preparation of chitin-beta-cyclodextrin resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490349A (en) * | 2002-10-15 | 2004-04-21 | 浙江大学 | Preparation of chitin-beta-cyclodextrin resin |
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Non-Patent Citations (1)
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| 《壳聚糖基功能材料的制备及性能测定》;张文清等;《壳聚糖基功能材料的制备及性能测定》;20100630;第36卷(第3期);402页 * |
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