CN110314660A - Modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method and products thereof and application - Google Patents
Modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method and products thereof and application Download PDFInfo
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- CN110314660A CN110314660A CN201910635568.3A CN201910635568A CN110314660A CN 110314660 A CN110314660 A CN 110314660A CN 201910635568 A CN201910635568 A CN 201910635568A CN 110314660 A CN110314660 A CN 110314660A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The present invention relates to a kind of modification of chitosan-nano silicon dioxide hybridization adsorbent preparation methods and products thereof and application, and preparation method includes: the purifying of nano-silica surface functionalization, the preparation of hybrid sorbents and hybrid sorbents.Compared with prior art, chitosan source used in the present invention is wide, cheap, and product can be biodegradable completely, therefore will not cause secondary pollution to environment.Using Nano-meter SiO_22Particle surface has the characteristics that silanol hydroxy groups group and large specific surface area, realizes Nano-meter SiO_22With sufficiently reacting for epoxychloropropane, the SiO of hydroxypropyl chlorination is obtained2Particle；Cross-linking is fixed on chitosan again, is prepared for novel chitosan-Nano-meter SiO_2 with chemical bonds2Hydridization adsorbent material.The advantages that adsorbent has adsorption effect good, and sinking speed is fast, and preparation is simple, safety and environmental protection.
Description
Technical field
The present invention relates to field of waste water treatment, specifically a kind of modification of chitosan-nano silicon dioxide hybridization adsorbent
Preparation method and products thereof and application.
Background technique
Absorption method is one of important method of wastewater treatment, and sewage also remains in water outlet after conventional wastewater treatment
Hardly degraded organic substance, free chlorine and some trace meters such as mercury, silver, chromium, antimony, arsenic, using absorption method can remove it is most of these
Substance.The detersive efficiency of absorption method, cost are largely different because of adsorbent difference, and the most common adsorbent is activity
Charcoal.Absorption method is not also very much, but the research of nearly more than ten years at home for the theoretical research studies in China achievement of sewage treatment
In, the research of adsorbent accounts for very big ratio.
Chitosan is a kind of natural polymer, and abundance has non-toxic and tasteless, adsorptivity and biocompatible
The features such as property is good, has been widely used in adsorbing domain.Also, due to the cellular structure of chitosan and free amino, hydroxyl
In the presence of, can effectively adsorb and capture metal ions, form stable chelate, have been considered as removing from sewage metal from
The best candidate material of son.
But chitosan is as adsorbent, there are density it is small, the rate of settling is slow the disadvantages of.Overcome disadvantages mentioned above, it is a kind of
Method is to synthesize chitosan microball by crosslinking agent；Another method is synthesizing organic-inorganic hybrid material.
Hybrid inorganic-organic materials are as a kind of novel material, with polymer gel and inorganic nano-particle
Good characteristic, such as high resiliency, high swelling property, high intensity and deswelling rate be fast.In recent years, with silica and high score
Common concern of the composite organic-inorganic material that sub- compound hydridization is formed by domestic and international researcher.
Summary of the invention
In view of the deficiencies of the prior art, present invention aims at: a kind of modification of chitosan-nano silicon dioxide hybridization is provided
The preparation method of adsorbent.
Another object of the present invention is: providing the product that the preparation method obtains.
Another object of the present invention is to: the application of the product is provided.
The object of the invention is realized by following proposal: a kind of system of modification of chitosan-nano silicon dioxide hybridization adsorbent
Preparation Method utilizes Nano-meter SiO_22Particle surface has the characteristics that silanol hydroxy groups group and large specific surface area, realizes Nano-meter SiO_22
With sufficiently reacting for epoxychloropropane, the SiO of hydroxypropyl chlorination is obtained2Particle；Cross-linking is fixed on chitosan again, preparation
At with chitosan-Nano-meter SiO_2 of chemical bonds2Hydridization adsorbent material, including following preparation step:
(1) nano-silica surface functionalization
Weigh a certain amount of Nano-meter SiO_22Acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts molten
The pH of liquid is to being not more than 5, then weighs epoxychloropropane, is added dropwise dropwise with dropping funel, makes SiO2Particle, acetone, epoxy chloropropionate
The mass ratio of alkane is 1:(17-25): (5-9) after being added dropwise, loads onto reflux condensing tube and completes after heating reaction, be cooled to room
Temperature, evaporative removal solvent obtains white solid powder, and product is vacuum dried, obtains the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
A certain amount of chitosan, sodium hydroxide and isopropanol are weighed into three-necked flask, makes chitosan, sodium hydroxide, isopropanol
Mass ratio be 10:(1-3): (200-280) is sufficiently stirred and is placed in (40-60) DEG C water bath with thermostatic control after quaternization, Xiang Rong
The SiO of appropriate hydroxypropyl chlorination is added in liquid2Particle makes the SiO of chitosan, hydroxypropyl chlorination2The mass ratio of particle is 1:(1-
2) it, after the completion of isothermal reaction, is cooled to room temperature, filters, filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purification process the purifying of hybrid sorbents: is carried out to hybrid sorbents.
Wherein, in step (1): pH range are as follows: (3-5)；Heat reaction temperature are as follows: (60-80) DEG C；Reaction time are as follows: (6-
10) h.
In step (2): alkalization time are as follows: (2-6) h；Chitosan, hydroxypropyl chlorination SiO2The reaction time of particle are as follows:
(3-7) h.
Purification process is carried out to hybrid sorbents:
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, finally obtains the modification of purifying
Chitosan-nano silicon dioxide hybridization adsorbent product.
The principle of the invention is: utilizing Nano-meter SiO_22Particle surface has the spy of silanol hydroxy groups group and large specific surface area
Point, realizes Nano-meter SiO_22With sufficiently reacting for epoxychloropropane, the SiO of hydroxypropyl chlorination is obtained2Particle；Cross-linking is solid again
It is scheduled on chitosan, is prepared for novel chitosan-Nano-meter SiO_2 with chemical bonds2Hydridization adsorbent material.
The present invention also provides a kind of hydridization adsorbent material products obtained according to above-mentioned preparation method.
The hydridization adsorbent material overcomes chitosan and haves the shortcomings that settling rate is slow separately as adsorbent, effectively ties
The flexibility of chitosan and the rigidity of silica have been closed, the reunion of nano SiO 2 particle has been avoided, can not only increase shell
The specific surface area and density of glycan, and the absorption property and the rate of settling of chitosan can be improved.
Present invention provides the applications of the said goods.
Chitosan as a kind of environment-friendly material, have it is from a wealth of sources, safe and non-toxic, cheap, be easy to biological drop
Solution and the outstanding features such as environmental-friendly；Nano silica has porous, certain chemical inertness, higher specific surface area and heat
The features such as stability；Chitosan and nanometer silicon dioxide particle can be formed good dispersion with it is compatible；By the titanium dioxide of functionalization
Nano silicon particles are fixed on chitosan with chemical bond crosslinking, have been effectively combined the flexible and silica rigid of chitosan
Property, the reunion of nano SiO 2 particle is avoided, the specific surface area and density of chitosan can be not only increased, but also can be improved
The absorption property and the rate of settling of chitosan.The adsorbent has adsorption effect good, and sinking speed is fast, and preparation is simple, safety collar
The advantages that guarantor.
Compared with prior art, chitosan source used in the present invention is wide, cheap, and product can quilt completely
Biodegrade, therefore secondary pollution will not be caused to environment.Using Nano-meter SiO_22Particle surface have silanol hydroxy groups group and
The characteristics of large specific surface area, realizes Nano-meter SiO_22With sufficiently reacting for epoxychloropropane, the SiO of hydroxypropyl chlorination is obtained2?
Grain；Cross-linking is fixed on chitosan again, is prepared for novel chitosan-Nano-meter SiO_2 with chemical bonds2Hydridization absorption
Material.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of modification of chitosan-nano silicon dioxide hybridization adsorbent, which is characterized in that utilize Nano-meter SiO_22?
Grain surface has the characteristics that silanol hydroxy groups group and large specific surface area, realizes Nano-meter SiO_22It is abundant anti-with epoxychloropropane
It answers, obtains the SiO of hydroxypropyl chlorination2Particle；Cross-linking is fixed on chitosan again, is prepared into poly- with the shell of chemical bonds
Sugar-Nano-meter SiO_22Hydridization adsorbent material, is prepared as follows step:
(1) nano-silica surface functionalization
Weigh the Nano-meter SiO_2 of 10g2170g acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts
PH=3 of solution, then 50g epoxychloropropane is weighed, it is added dropwise dropwise with dropping funel, after being added dropwise, loads onto reflux condensing tube and add
Heat to 60 DEG C of reactions are cooled to room temperature, evaporative removal solvent obtains white solid powder, and product is done through vacuum after reacting 10h
It is dry, obtain the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
The chitosan, 0.5g sodium hydroxide and 100g isopropanol of 5g are weighed into three-necked flask, is sufficiently stirred and is placed on 40 DEG C of perseverances
In tepidarium, the SiO of 5g hydroxypropyl chlorination is added into solution by constant temperature alkalization 6h2Particle after isothermal reaction 3h, is cooled to room
Temperature, filters, and filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, obtains final modification of chitosan-
Nano silicon dioxide hybridization adsorbent product.
Certain steel plant wastewater is handled with prepared modification of chitosan-nano silicon dioxide hybridization adsorbent, is given up
The initial COD value of water is 405 mg/L, and the dosage of flocculant is 6 ‰, by 10 minutes flocculation sedimentations, the removal rate of COD
It is 57.6%.
Embodiment 2
A kind of preparation method of modification of chitosan-nano silicon dioxide hybridization adsorbent, step is prepared as follows:
(1) nano-silica surface functionalization
Weigh the Nano-meter SiO_2 of 10g2190g acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts
PH=3.5 of solution, then 60g epoxychloropropane is weighed, it is added dropwise dropwise with dropping funel, after being added dropwise, loads onto reflux condensing tube
65 DEG C of reactions are heated to be cooled to room temperature, evaporative removal solvent obtains white solid powder, by product through vacuum after reacting 9h
It is dry, obtain the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
The chitosan, 0.75g sodium hydroxide and 110g isopropanol of 5g are weighed into three-necked flask, is sufficiently stirred and is placed on 45 DEG C of perseverances
In tepidarium, the SiO of 6g hydroxypropyl chlorination is added into solution by constant temperature alkalization 5h2Particle after isothermal reaction 4h, is cooled to room
Temperature, filters, and filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, obtains final products；
Certain steel plant wastewater is handled with prepared modification of chitosan-nano silicon dioxide hybridization adsorbent, waste water
Initial COD value is 405 mg/L, and the dosage of flocculant is 6 ‰, and by 10 minutes flocculation sedimentations, the removal rate of COD was
54.9%。
Embodiment 3
A kind of preparation method of modification of chitosan-nano silicon dioxide hybridization adsorbent, step is prepared as follows:
(1) nano-silica surface functionalization
Weigh the Nano-meter SiO_2 of 10g2210g acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts
PH=4 of solution, then 70g epoxychloropropane is weighed, it is added dropwise dropwise with dropping funel, after being added dropwise, loads onto reflux condensing tube and add
Heat to 70 DEG C of reactions are cooled to room temperature, evaporative removal solvent obtains white solid powder, and product is done through vacuum after reacting 8h
It is dry, obtain the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
The chitosan, 1g sodium hydroxide and 120g isopropanol of 5g are weighed into three-necked flask, is sufficiently stirred and is placed on 50 DEG C of constant temperature
In water-bath, the SiO of 7g hydroxypropyl chlorination is added into solution by constant temperature alkalization 4h2Particle after isothermal reaction 5h, is cooled to room temperature,
It filters, filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, obtains final products.
Certain steel plant wastewater is handled with prepared modification of chitosan-nano silicon dioxide hybridization adsorbent, is given up
The initial COD value of water is 405 mg/L, and the dosage of flocculant is 6 ‰, by 10 minutes flocculation sedimentations, the removal rate of COD
It is 56.1%.
Embodiment 4
A kind of preparation method of modification of chitosan-nano silicon dioxide hybridization adsorbent, step is prepared as follows:
(1) nano-silica surface functionalization
Weigh the Nano-meter SiO_2 of 10g2230g acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts
PH=4.5 of solution, then 80g epoxychloropropane is weighed, it is added dropwise dropwise with dropping funel, after being added dropwise, loads onto reflux condensing tube
75 DEG C of reactions are heated to be cooled to room temperature, evaporative removal solvent obtains white solid powder, by product through vacuum after reacting 7h
It is dry, obtain the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
The chitosan, 1.25g sodium hydroxide and 130g isopropanol of 5g are weighed into three-necked flask, is sufficiently stirred and is placed on 55 DEG C of perseverances
In tepidarium, the SiO of 9g hydroxypropyl chlorination is added into solution by constant temperature alkalization 3h2Particle after isothermal reaction 6h, is cooled to room
Temperature, filters, and filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, obtains final products；
Certain steel plant wastewater is handled with prepared modification of chitosan-nano silicon dioxide hybridization adsorbent, waste water
Initial COD value is 405 mg/L, and the dosage of flocculant is 6 ‰, and by 10 minutes flocculation sedimentations, the removal rate of COD was
53.7%。
Embodiment 5
A kind of preparation method of modification of chitosan-nano silicon dioxide hybridization adsorbent, step is prepared as follows:
(1) nano-silica surface functionalization
Weigh the Nano-meter SiO_2 of 10g2250g acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts
PH=5 of solution, then 90g epoxychloropropane is weighed, it is added dropwise dropwise with dropping funel, after being added dropwise, loads onto reflux condensing tube and add
Heat to 80 DEG C of reactions are cooled to room temperature, evaporative removal solvent obtains white solid powder, and product is done through vacuum after reacting 6h
It is dry, obtain the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
The chitosan, 1.5g sodium hydroxide and 140g isopropanol of 5g are weighed into three-necked flask, is sufficiently stirred and is placed on 60 DEG C of perseverances
In tepidarium, the SiO of 10g hydroxypropyl chlorination is added into solution by constant temperature alkalization 2h2Particle after isothermal reaction 7h, is cooled to room
Temperature, filters, and filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents
Hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter sealing is placed on
In 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, is finally determined with silver nitrate aqueous solution thick
Whether sodium chloride has eliminated in product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, obtains final products；
Certain steel plant wastewater is handled with prepared modification of chitosan-nano silicon dioxide hybridization adsorbent, waste water
Initial COD value is 405 mg/L, and the dosage of flocculant is 6 ‰, and by 10 minutes flocculation sedimentations, the removal rate of COD was
56.6%。
Claims (6)
1. a kind of modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method, which is characterized in that utilize Nano-meter SiO_22
Particle surface has the characteristics that silanol hydroxy groups group and large specific surface area, realizes Nano-meter SiO_22It is abundant with epoxychloropropane
Reaction, obtains the SiO of hydroxypropyl chlorination2Particle；Cross-linking is fixed on chitosan again, is prepared into the shell with chemical bonds
Glycan-Nano-meter SiO_22Hydridization adsorbent material, including following preparation step:
(1) nano-silica surface functionalization
Weigh a certain amount of Nano-meter SiO_22Acetone is added in three-necked flask in particle, and dilute hydrochloric acid is added dropwise in stirring while, adjusts molten
The pH of liquid is to being not more than 5, then weighs epoxychloropropane, is added dropwise dropwise with dropping funel, makes SiO2Particle, acetone, epoxy chloropropionate
The mass ratio of alkane is 1:(17-25): (5-9) after being added dropwise, loads onto reflux condensing tube heating after the reaction was completed, is cooled to room
Temperature, evaporative removal solvent obtains white solid powder, and product is vacuum dried, obtains the SiO of hydroxypropyl chlorination2Particle；
(2) preparation of hybrid sorbents
A certain amount of chitosan, sodium hydroxide and isopropanol are weighed into three-necked flask, makes chitosan, sodium hydroxide, isopropanol
Mass ratio be 10:(1-3): (200-280), be sufficiently stirred be placed in (40-60) DEG C water bath with thermostatic control alkalize after, into solution
The SiO of appropriate hydroxypropyl chlorination is added2Particle makes the SiO of chitosan, hydroxypropyl chlorination2The mass ratio of particle is 1:(1-2), it is permanent
Temperature after the reaction was completed, is cooled to room temperature, and is filtered, and filter cake distilled water flushing obtains hybrid sorbents after vacuum drying；
(3) purifying of hybrid sorbents.
2. modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method, feature exist according to claim 1
In: in step (1): pH 3-5；Reflux condensing tube heats reaction temperature are as follows: (60-80) DEG C, reaction time are as follows: (6-10) h.
3. modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method, feature exist according to claim 1
In: in step (2): alkalization time are as follows: (2-6) h；Chitosan, hydroxypropyl chlorination SiO2Particle isothermal reaction (3-7) h.
4. modification of chitosan-nano silicon dioxide hybridization adsorbent preparation method, feature exist according to claim 1
In: in step (3): hybrid sorbents are fitted into the bag filter that the relative molecular mass that shuts off is 2000 or more, bag filter is close
It is honored as a queen and is placed in 500mL deionized water, dialyse 15h under magnetic stirring, changes a water every 5h, finally uses silver nitrate aqueous solution
To determine, whether sodium chloride has been eliminated in crude product；The hybrid sorbents vacuum drying of sodium chloride will be eliminated, is finally produced
Product.
5. a kind of modification of chitosan-nano silicon dioxide hybridization adsorbent, it is characterised in that -4 is any described according to claim 1
Method is prepared.
6. a kind of modification of chitosan-nano silicon dioxide hybridization adsorbent according to claim 5 is at the waste water of ironworks
Application in reason.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111659354A (en) * | 2020-06-18 | 2020-09-15 | 威海海洋职业学院 | Hydroxyl graphene-nano silicon dioxide modified chitosan composite material and application thereof |
| CN114106651A (en) * | 2021-12-13 | 2022-03-01 | 瑞氟涂料科技(南雄)有限公司 | High-temperature-resistant fluorine-silicon coating and preparation method thereof |
| CN114752002A (en) * | 2022-04-06 | 2022-07-15 | 东莞理工学院 | Organic modified chitosan adsorbent for removing PFASs, preparation method and application |
| CN117756459A (en) * | 2023-12-25 | 2024-03-26 | 万特福建筑构件有限公司 | Environment-friendly concrete and preparation method thereof |
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| CN111659354A (en) * | 2020-06-18 | 2020-09-15 | 威海海洋职业学院 | Hydroxyl graphene-nano silicon dioxide modified chitosan composite material and application thereof |
| CN114106651A (en) * | 2021-12-13 | 2022-03-01 | 瑞氟涂料科技(南雄)有限公司 | High-temperature-resistant fluorine-silicon coating and preparation method thereof |
| CN114752002A (en) * | 2022-04-06 | 2022-07-15 | 东莞理工学院 | Organic modified chitosan adsorbent for removing PFASs, preparation method and application |
| CN117756459A (en) * | 2023-12-25 | 2024-03-26 | 万特福建筑构件有限公司 | Environment-friendly concrete and preparation method thereof |
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