CN103691411A - Formaldehyde adsorbent containing chitosan and beta-cyclodextrin and preparation method for formaldehyde adsorbent - Google Patents
Formaldehyde adsorbent containing chitosan and beta-cyclodextrin and preparation method for formaldehyde adsorbent Download PDFInfo
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- CN103691411A CN103691411A CN201410012978.XA CN201410012978A CN103691411A CN 103691411 A CN103691411 A CN 103691411A CN 201410012978 A CN201410012978 A CN 201410012978A CN 103691411 A CN103691411 A CN 103691411A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 239000003463 adsorbent Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920000858 Cyclodextrin Polymers 0.000 title abstract description 12
- 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 title abstract description 7
- 229920001661 Chitosan Polymers 0.000 title abstract 7
- 239000001116 FEMA 4028 Substances 0.000 title abstract 5
- 235000011175 beta-cyclodextrine Nutrition 0.000 title abstract 5
- 229960004853 betadex Drugs 0.000 title abstract 5
- 239000000243 solution Substances 0.000 claims abstract description 26
- 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 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 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
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 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
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 235000019256 formaldehyde Nutrition 0.000 description 26
- 238000010521 absorption reaction Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 8
- 238000003795 desorption Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229930040373 Paraformaldehyde Natural products 0.000 description 4
- 230000004087 circulation Effects 0.000 description 4
- 229920002866 paraformaldehyde Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 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
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 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
- 230000002349 favourable 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Abstract
The invention discloses a formaldehyde adsorbent containing chitosan and beta-cyclodextrin and a preparation method for the formaldehyde adsorbent. The formaldehyde adsorbent is prepared from the chitosan and the beta-cyclodextrin; the mass ratio of the chitosan to the beta-cyclodextrin is (1:4)-(1:8). The preparation method comprises the steps of dissolving the chitosan in hydrochloric acid; mixing and stirring the dissolved chitosan with the beta-cyclodextrin solution; slowly dropping a glutaraldehyde solution into the mixed solution, and heating and stirring the mixed solution under the protection of inert gas; adding a sodium hydroxide solution into the reaction solution to separate out products, filtering the products, washing the products through water until the products are neutralized, and then washing the neutralized products through acetone; and performing vacuum drying. By the integration of the identification performance of the cyclodextrin and the adsorption function of the chitosan, the formaldehyde adsorbent is high in adsorption performance, stable in property, high in reproducibility and high in selectivity; the content of formaldehyde gas in a space can be greatly reduced; furthermore, the adsorbent preparation technology is simple, the cost is low, and pollution is avoided; the preparation method is suitable for industrial production.
Description
Technical field
The invention belongs to sorbing material preparation and application, specifically, relate to a kind of formaldehyde adsorbent and preparation method thereof.
Background technology
Formaldehyde claims again formaldehyde, has intense stimulus smell, is a kind of important healthy indoor air pollutants of harm people.Along with social progress, 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.Purifying formaldehyde technology in research room air, improves IAQ, has very important significance.
Method for air methanal removing has absorption method, catalytic oxidation, biological degradation method, plasma technique etc. at present.These methods respectively have pluses and minuses, and wherein the most frequently used be absorption method.Take at present all kinds of active carbons and goods thereof is that main solid absorbent only has more intense suction-operated to the material of nonpolar or low pole, and very little to the formaldehyde absorbing capacity of strong polarity, and easily by secondary, discharged in the situation that the saturated and temperature of absorption is higher.Therefore, need badly exploitation cheaply a kind of, 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, has two kinds of reactive groups of abundant amino and hydroxyl on strand, can interact with the aldehyde radical of formaldehyde, for the indoor free formaldehyde of adsorption removal.CN 101327424A discloses a kind of with shitosan, and manganese dioxide and active carbon evenly mix the Powdered formaldehyde adsorbent making.Beta-schardinger dextrin-(β-CD) has special molecular structure and a plurality of chiral molecules of " interior hydrophobic, outer hydrophilic ", can be used as different " object " compounds of " host " envelope, forms the special inclusion complex of structure.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.Cyclodextrin is immobilized to shitosan, not only combine recognition performance and the shitosan absorption property of cyclodextrin, stability and absorption property that can also reinforcing material.At present, there is no the immobilized β-CD of shitosan as the relevant report of solid-phase gas pollutant absorbent.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of formaldehyde adsorbent that contains shitosan and beta-schardinger dextrin-and preparation method thereof is provided.
For achieving the above object, the present invention adopts following technical scheme:
A formaldehyde adsorbent, is made by shitosan and beta-schardinger dextrin-, and shitosan and beta-schardinger dextrin-mass ratio are 1: 4 ~ 1: 8.
The preparation method of above-mentioned formaldehyde adsorbent, comprises the steps:
Step 1, shitosan is dissolved in hydrochloric acid solution, then with beta-schardinger dextrin-solution by volume 1:1 mix, stir under room temperature;
Step 2, toward in the mixed solution obtaining in step 1 in mixed liquor: the glutaraldehyde solution volume ratio ratio of 10: 1 ~ 50: 1, speed with 0.1 ~ 1.0 mL/min drips glutaraldehyde solution, and at inert gas shielding and 50 ~ 80 ℃, stir 1 ~ 24 hour;
Step 3, in the mixed solution obtaining in step 2, add sodium hydroxide solution that product is separated out, filter and wash with water product to neutral, then with acetone washing, vacuum drying is stable to product quality at 60 ℃;
Step 4, the solid product that obtains in step 3 is pulverized, is sieved into the adsorbent of variable grain size, sealing saves backup.
In above-mentioned preparation method, the concentration of hydrochloric acid solution is 0.05 ~ 0.5 mol/L described in step 1, and the mass fraction of glutaraldehyde solution is 15% ~ 25% described in step 2.
In above-mentioned preparation method, the concentration of sodium hydroxide solution is 0.5 ~ 3 mol/L described in step 3, with the volume ratio of mixed liquor be 1: 3 ~ 1: 8.
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, selectively good, can greatly 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.
The specific embodiment
Embodiment 1: the preparation of the immobilized beta-schardinger dextrin-adsorbent of shitosan:
Step 1,4 g shitosans are dissolved in to 200 mL concentration is in the hydrochloric acid of 0.1 mol/L, and the cyclodextrin solution that adds 200 mL to contain 24 g beta-schardinger dextrin-s;
Step 2, the mixed liquor obtaining in step 1 is stirred after 1 h at 25 ℃, the speed of 0.8mL/min of take drips the glutaraldehyde solution that 24 mL concentration are 25%;
Step 3, by the mixed liquor obtaining in step 2 at nitrogen protection and 70 ℃, stop reaction after stirring 6 h;
Step 4, the sodium hydroxide solution that is 1 mol/L by 70 mL concentration join in the mixed liquor obtaining in step 3 product are separated out, and filter, and wash with water to neutrality and wash with acetone, and finally at 60 ℃, vacuum drying is stable to product quality;
Step 5, the solid product obtaining in step 4 is sieved into the adsorbent that granular size is 0.20 ~ 0.45 mm, sealing saves backup.
Embodiment 2: the preparation of the immobilized beta-schardinger dextrin-adsorbent of shitosan:
Step 1,4 g shitosans are dissolved in to 150 mL concentration is in the hydrochloric acid of 0.2 mol/L, and the cyclodextrin solution that adds 150 mL to contain 16 g beta-schardinger dextrin-s;
Step 2, the mixed liquor obtaining in step 1 is stirred after 1 h at 25 ℃, the speed of 1 mL/min of take drips the glutaraldehyde solution that 30 mL concentration are 20%;
Step 3, by the mixed liquor obtaining in step 2 at nitrogen protection and 70 ℃, stop reaction after stirring 6 h;
Step 4, the sodium hydroxide solution that is 1 mol/L by 70 mL concentration join in the mixed liquor obtaining in step 3 product are separated out, and filter, and wash with water to neutrality and wash with acetone, and finally at 60 ℃, vacuum drying is stable to product quality;
Step 5, the solid product obtaining in step 4 is sieved into the adsorbent that granular size is 0.20 ~ 0.45 mm, sealing saves backup.
Embodiment 3: the absorption property of the adsorbent PARA FORMALDEHYDE PRILLS(91,95) of embodiment 1
By dynamic experiment method, investigated the absorption property of adsorbent PARA FORMALDEHYDE PRILLS(91,95).At ambient temperature, get 0.5 g and put into by the made adsorbent of embodiment 1 adsorption column that internal diameter is 7 mm, using air as carrier gas, by Bubbling method to the adsorbent bed formaldehyde that passes into.In air speed, be 1000 h
-1, air inlet concentration of formaldehyde is 46 mg/m
3time, the equilibrium adsorption capacity of formaldehyde is 13 mg (formaldehyde)/g (adsorbent).Adsorb saturated after, at 60 ℃, the air that directly passes into 100 mL/min purges desorption, formaldehyde desorption rate is greater than 98%, completes once absorption/desorption circulation.After three circulations, the adsorbance of formaldehyde is 12 mg (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 the adsorbent of embodiment 2 preparations, and the equilibrium adsorption capacity of formaldehyde is 11 mg (formaldehyde)/g (adsorbent).Adsorb saturated after, at 60 ℃, the air that directly passes into 100 mL/min purges desorption, formaldehyde desorption rate is greater than 98%, completes once absorption/desorption circulation.After three circulations, the adsorbance of formaldehyde is 10.2 mg (formaldehyde)/g (adsorbent), illustrates that the immobilized beta-schardinger dextrin-adsorbent of shitosan can be recycled.
Claims (4)
1. a formaldehyde adsorbent, is characterized in that being made by shitosan and beta-schardinger dextrin-, and shitosan and beta-schardinger dextrin-mass ratio are 1: 4 ~ 1: 8.
2. the preparation method of formaldehyde adsorbent described in claim 1, is characterized in that, comprises the steps:
Step 1, shitosan is dissolved in hydrochloric acid solution, then with beta-schardinger dextrin-solution by volume 1:1 mix, stir under room temperature;
Step 2, toward in the mixed solution obtaining in step 1 in mixed liquor: the glutaraldehyde solution volume ratio ratio of 10: 1 ~ 50: 1, speed with 0.1 ~ 1.0 mL/min drips glutaraldehyde solution, and at inert gas shielding and 50 ~ 80 ℃, stir 1 ~ 24 hour;
Step 3, in the mixed solution obtaining in step 2, add sodium hydroxide solution that product is separated out, filter and wash with water product to neutral, then with acetone washing, vacuum drying is stable to product quality at 60 ℃;
Step 4, the solid product that obtains in step 3 is pulverized, is sieved into the adsorbent of variable grain size, sealing saves backup.
3. preparation method according to claim 2, is characterized in that, the concentration of hydrochloric acid solution is 0.05 ~ 0.5 mol/L described in step 1, and the mass fraction of glutaraldehyde solution is 15% ~ 25% described in step 2.
4. preparation method according to claim 2, is characterized in that, the concentration of sodium hydroxide solution is 0.5 ~ 3 mol/L described in step 3, with the volume ratio of mixed liquor be 1: 3 ~ 1: 8.
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| CN201410012978.XA CN103691411B (en) | 2014-01-13 | 2014-01-13 | A kind of formaldehyde adsorbent containing shitosan and beta-schardinger dextrin-and preparation method thereof |
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| CN201410012978.XA CN103691411B (en) | 2014-01-13 | 2014-01-13 | A kind of formaldehyde adsorbent containing shitosan and beta-schardinger dextrin-and preparation method thereof |
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| CN103691411B CN103691411B (en) | 2016-04-13 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| TWI483773B (en) * | 2014-04-09 | 2015-05-11 | Prior Company Ltd | Aqueous formaldehyde scavenger composition |
| 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 |
| 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 |
| 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 |
| 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 |
| CN114208848A (en) * | 2022-01-20 | 2022-03-22 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| 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 |
| CN114208848A (en) * | 2022-01-20 | 2022-03-22 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods 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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| CN103691411B (en) | 2016-04-13 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160413 |