CN107552010A - A kind of preparation method of titanium silicate chitosan absorbent - Google Patents
A kind of preparation method of titanium silicate chitosan absorbent Download PDFInfo
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Abstract
A kind of preparation method of titanium silicate chitosan absorbent disclosed by the invention, prepares the spherical titanium silicate in ultra-fine hole first, then is carried on chitosan molecule bead and titanium silicate chitosan absorbent is made；Present invention employs natural polymerses --- and chitosan is as functive, acid is melted into by the use of it and the Chitosan Beads of the preferable nanometer titanium silicate of characteristic combination adsorption capacity insoluble in alkali are used as sorbing material, there is provided a kind of preparation method for the synthetic adsorbent that easy-to-use absorption property is good, high mechanical strength, regeneration temperature are low.
Description
Technical field
The invention belongs to the fabricating technology field of solids containing titanium adsorbent composition, is related to a kind of titanium silicate chitosan
The preparation method of adsorbent.
Background technology
Perfluorochemical (PFCs) has very unique physicochemical properties such as hydro-oleophobicity, is widely used in
In industry, business and individual consumer's goods.The stability of perfluorochemical is very strong, has antiacid, alkali resistant, antioxidant and anti-reduction
The ability of agent, be typically resistant to hydrolyze, photodissociation, biodegradation etc..In addition, perfluorochemical (such as PFOA and PFOS) can be with
Accumulated by food chain, influence biological cell membrane characteristics, peroxisome proliferation, endocrine function, nurture, reproduction
Ability, lipid metabolism and enzymatic activity etc..It thus is seen that perfluorochemical belongs to PBT class materials, i.e., with persistence, biology product
Tired property and toxicity.
Chitin is widespread in nature to be moved in arthropod, mollusk, annelid, protozoan, coelenteron
It is the second largest renewable resource that yield is only second to cellulose on the earth in the organisms such as thing, marine alga and fungi.Chitosan
(chitosan, poly- (1,4) -2- amino -2- deoxidations-β-D-Glucose) is obtained by chitin by deacetylation
A kind of natural polymerses, it is however generally that, the can of N-acetyl group de- more than 55% is referred to as chitosan.
With the development of nanometer technology so that synthesize the low adsorbent material of good absorption property, high mechanical strength, regeneration temperature
Material, there is new favourable turn so as to produce the low efficient depth dehumidification equipment of small volume, energy consumption.
If their special molecule distinguishabilities can be combined with the preferable nanometer technology of adsorption capacity, it should energy
Enough solves the problems, such as the selective absorption degraded of target contaminant.
The content of the invention
It is an object of the invention to provide a kind of preparation method of titanium silicate chitosan absorbent, solves existing adsorbent
The problem of absorption property is weaker, mechanical strength is relatively low and molecule distinguishability is weaker.
The technical solution adopted in the present invention is a kind of preparation method of titanium silicate chitosan absorbent,
Specifically implement according to following steps：
The preparation of step 1, the spherical titanium silicate in ultra-fine hole：
First allowing silicon alkoxide/ethanol solution partial hydrolysis, then heating adds Titanium alkoxides/ethanol solution, allows its complete hydrolysis,
Adding polymeric additive polyethylene glycol makes its polycondensation and is aged colloidal sol is made, and water-setting is made through oil-free forming technique in colloidal sol
Glue, the spherical titanium silicate of nano aperture is made after scrubbed, dry and screening；
Step 2, load titanium silicate Chitosan Beads adsorbent preparation：
Titanium silicate made from step 1 is added in chitosan solution, carrying out ultrasonic wave after well mixed disperses, and adds afterwards
Epoxychloropropane and OP emulsifying agents, and stir, alkaline solution is continuously added, forms the Chitosan Beads of load titanium silicate,
And the Chitosan Beads for loading titanium silicate are put into alkaline solution after immersion, cleaned with distilled water, afterwards by Chitosan Beads
It is put into sodium hydroxide solution, and is stirred 4~6 hours at 25 DEG C, then clear is washed with deionized water to the shell of load titanium silicate
Glycan bead adsorbent.
The features of the present invention also resides in：
The preparation of colloidal sol in step 1 specifically comprises the following steps：Quality point is instilled into deionized water under ice-water bath
Number is in 20%~40% silicon alkoxide/ethanol solution, after reacting 30min~45min, is warming up to 40 DEG C~60 DEG C, adds matter
Titanium alkoxides/ethanol solution that fraction is 20%~40% is measured, is stirred, continuing dropwise addition acid solution is fully hydrolyzed it, reacts
After 70min~100min, the polyethylene glycol for accounting for silicon alkoxide and Titanium alkoxides total moles fraction 0.3%~0.6% is added, continues to react
After 50min~70min, stable sol can be formed by being aged 5d~10d at room temperature.
The mol ratio of silicon alkoxide and Titanium alkoxides is 8~20.
The preparation of the spherical titanium silicate of nano aperture specifically comprises the following steps：Using oil-free forming technique, pH value is adjusted
Colloidal sol is set to be solidified into hydrogel in atmosphere, it is scrubbed, 17h~21h is dried at a temperature of 120 DEG C~145 DEG C, is then sieved
Point, and the micelle after screening in accordance with granularity requirements is subjected to redrying, 130 DEG C~160 DEG C of drying temperature, drying time 21h
~25h, moisture are controlled below 2%, that is, prepare the spherical titanium silicate of nano aperture.
The mass ratio of titanium silicate and chitosan is 1 in step 2：3~5.
Chitosan mass and epoxychloropropane volume ratio are 1 in step 2：3~5g/ml, added chitosan mass and OP breasts
Agent volume ratio is 1：2~3g/ml.
The Chitosan Beads for loading titanium silicate are put into alkaline solution in step 2 and soak at least 10h.
The beneficial effects of the invention are as follows：
A kind of preparation method of titanium silicate chitosan absorbent of the present invention, employs natural polymerses --- and shell gathers
Sugar be used as functive, and sour and the preferable nanometer titanium silicate of characteristic combination adsorption capacity insoluble in alkali chitosan is melted into using it
Bead is as sorbing material, there is provided the synthesis that a kind of easy-to-use absorption property is good, high mechanical strength, regeneration temperature are low is inhaled
Attached dose of preparation method；The orientable absorption of the chitosan absorbent of titanium silicate produced by the present invention, efficient degradation perfluorochemical,
As a kind of new regenerable sorbent good effect can be played in perfluorochemical processing；In addition this preparation technology it is simple,
Cost is low, is with a wide range of applications.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of preparation method of titanium silicate chitosan absorbent, specifically implements according to following steps：
The preparation of step 1, the spherical titanium silicate in ultra-fine hole：
Instilled under ice-water bath into deionized water in silicon alkoxide/ethanol solution that mass fraction is 20%~40%, instead
After answering 30min~45min, 40 DEG C~60 DEG C are warming up to, is 8~20 according to the mol ratio of silicon alkoxide and Titanium alkoxides, adds quality
Fraction is 20%~40% Titanium alkoxides/ethanol solution, is stirred, and continuing dropwise addition acid solution is fully hydrolyzed it, reacts
After 70min~100min, the polyethylene glycol for accounting for silicon alkoxide and Titanium alkoxides total moles fraction 0.3%~0.6% is added, continues to react
After 50min~70min, stable sol can be formed by being aged 5d~10d at room temperature；Using oil-free forming technique, pH value is adjusted
Colloidal sol is set to be solidified into hydrogel in atmosphere, it is scrubbed, 17h~21h is dried at a temperature of 120 DEG C~145 DEG C, is then sieved
Point, and the micelle after screening in accordance with granularity requirements is subjected to redrying, 130 DEG C~160 DEG C of drying temperature, drying time 21h
~25h, moisture are controlled below 2%, that is, prepare the spherical titanium silicate of nano aperture.
Step 2, load titanium silicate Chitosan Beads adsorbent preparation：
It is 1 according to the mass ratio of titanium silicate and chitosan：3~5, silicic acid made from step 1 is added into chitosan solution
Titanium, carry out ultrasonic wave after well mixed and disperse, add epoxychloropropane and OP emulsifying agents afterwards, and stir, continuously add
Alkaline solution, the Chitosan Beads of load titanium silicate are formed, and the Chitosan Beads for loading titanium silicate are put into alkaline solution
After soaking at least 10h, cleaned with distilled water, Chitosan Beads are put into sodium hydroxide solution afterwards, and 4 are stirred at 25 DEG C
~6 hours, then clear is washed with deionized water to the Chitosan Beads adsorbent of load titanium silicate.
Wherein, chitosan mass and epoxychloropropane volume ratio are 1：3~5g/ml, added chitosan mass emulsify with OP
Agent volume ratio is 1：2~3g/ml.
Embodiment 1
Under ice-water bath, in the 500mL flasks equipped with magnetic stirring apparatus, dropping funel and reflux, 20% is added
TEOS ethanol solutions 250g (0.481mol), is uniformly mixed in dropping funel with 30.3mL deionized waters and slowly instills flask
In, after reacting 30 minutes, 40 DEG C are warming up to, by Si/Ti=12, adds 20%TBtOT ethanol solutions 34.1g (4.01 × 10- 2Mol), stir, continuing dropwise addition acid solution is fully hydrolyzed it, after further react 70 minutes, adds 1.25g PEG-
600(2.08×10-3Mol), continue reaction 50 minutes, be cooled to room temperature.Stable sol can be formed by being aged 5 days at 25 DEG C；
Regulation pH value makes colloidal sol be solidified into hydrogel in atmosphere, is filtered through 90 DEG C of deionized water detergent gels untill filtrate pH=7,
Dry 17 hours at a temperature of 120 DEG C, then sieved, the micelle after screening in accordance with granularity requirements carries out redrying, does
Dry 130 DEG C of temperature, 21 hours drying times, moisture control less than 2%, that is, prepare the granular titanium silicate of nano aperture；
From lobster shell extraction and deacetylation be 90% 0.5g chitosans be dissolved in 20ml 3% acetic acid solution be made
Chitosan solution, 0.17g titanium silicates are added into chitosan solution, and carrying out ultrasonic wave after well mixed disperses, and adds afterwards
1.5g epoxychloropropane and 1.0g OP emulsifying agents, and stir, alkaline solution is continuously added, forms load titanium silicate
Chitosan Beads, and after being put into alkaline solution by the Chitosan Beads for loading titanium silicate and soak at least 10h, washed with distillation
Only, Chitosan Beads are put into sodium hydroxide solution afterwards, and stirred 4 hours at 25 DEG C, then clear is washed with deionized water
To the Chitosan Beads adsorbent of load titanium silicate.
Embodiment 2
Under ice-water bath, in the 500mL flasks equipped with magnetic stirring apparatus, dropping funel and reflux, 25% is added
TEOS ethanol solutions 250g (0.481mol), is uniformly mixed in dropping funel with 30.3mL deionized waters and slowly instills flask
In, after reacting 35 minutes, 45 DEG C are warming up to, by Si/Ti=12, adds 25%TBtOT ethanol solutions 34.1g (4.01 × 10- 2Mol), stir, continuing dropwise addition acid solution is fully hydrolyzed it, after further react 80 minutes, adds 1.25g PEG-
600(2.08×10-3Mol), continue reaction 60 minutes, be cooled to room temperature；Stable sol can be formed by being aged 7 days at 25 DEG C；
Regulation pH value makes colloidal sol be solidified into hydrogel in atmosphere, is filtered through 90 DEG C of deionized water detergent gels untill filtrate pH=7,
Dry 18 hours at a temperature of 120 DEG C, then sieved, the micelle after screening in accordance with granularity requirements carries out redrying, does
Dry 140 DEG C of temperature, 23 hours drying times, moisture control less than 2%, that is, prepare the granular titanium silicate of nano aperture；
From lobster shell extraction and deacetylation be 90% 0.5g chitosans be dissolved in 20ml 3% acetic acid solution be made
Chitosan solution, 0.125g titanium silicates are added into chitosan solution, and carrying out ultrasonic wave after well mixed disperses, and adds afterwards
2.0g epoxychloropropane and 2.0g OP emulsifying agents, and stir, alkaline solution is continuously added, forms load titanium silicate
Chitosan Beads, and after being put into alkaline solution by the Chitosan Beads for loading titanium silicate and soak at least 10h, washed with distillation
Only, Chitosan Beads are put into sodium hydroxide solution afterwards, and stirred 5 hours at 25 DEG C, then clear is washed with deionized water
To the Chitosan Beads adsorbent of load titanium silicate.
Embodiment 3
Under ice-water bath, in the 500mL flasks equipped with magnetic stirring apparatus, dropping funel and reflux, 30% is added
TEOS ethanol solutions 250g (0.481mol), is uniformly mixed in dropping funel with 30.3mL deionized waters and slowly instills flask
In, after reacting 35 minutes, 45 DEG C are warming up to, by Si/Ti=12, adds 30%TBtOT ethanol solutions 34.1g (4.01 × 10- 2Mol), stir, continuing dropwise addition acid solution is fully hydrolyzed it, after further react 90 minutes, adds 1.25g PEG-
600(2.08×10-3Mol), continue reaction 65 minutes, be cooled to room temperature；Stable sol can be formed by being aged 8 days at 25 DEG C；
Regulation pH value makes colloidal sol be solidified into hydrogel in atmosphere, is filtered through 90 DEG C of deionized water detergent gels untill filtrate pH=7,
Dry 20 hours at a temperature of 130 DEG C, then sieved, the micelle after screening in accordance with granularity requirements carries out redrying, does
Dry 150 DEG C of temperature, 23 hours drying times, moisture control less than 2%, that is, prepare the granular titanium silicate of nano aperture；
From lobster shell extraction and deacetylation be 90% 0.5g chitosans be dissolved in 20ml 3% acetic acid solution be made
Chitosan solution, 0.125g titanium silicates are added into chitosan solution, and carrying out ultrasonic wave after well mixed disperses, and adds afterwards
2.5g epoxychloropropane and 2.0g OP emulsifying agents, and stir, alkaline solution is continuously added, forms load titanium silicate
Chitosan Beads, and after being put into alkaline solution by the Chitosan Beads for loading titanium silicate and soak at least 10h, washed with distillation
Only, Chitosan Beads are put into sodium hydroxide solution afterwards, and stirred 6 hours at 25 DEG C, then clear is washed with deionized water
To the Chitosan Beads adsorbent of load titanium silicate.
Embodiment 4
Under ice-water bath, in the 500mL flasks equipped with magnetic stirring apparatus, dropping funel and reflux, 35% is added
TEOS ethanol solutions 250g (0.481mol), is uniformly mixed in dropping funel with 30.3mL deionized waters and slowly instills flask
In, after reacting 40 minutes, 50 DEG C are warming up to, by Si/Ti=12, adds 35%TBtOT ethanol solutions 34.1g (4.01 × 10- 2Mol), stir, continuing dropwise addition acid solution is fully hydrolyzed it, after further react 95 minutes, adds 1.25g PEG-
600(2.08×10-3Mol), continue reaction 70 minutes, be cooled to room temperature；Stable sol can be formed by being aged 9 days at 25 DEG C；
Regulation pH value makes colloidal sol be solidified into hydrogel in atmosphere, is filtered through 90 DEG C of deionized water detergent gels untill filtrate pH=7,
Dry 20 hours at a temperature of 140 DEG C, then sieved, the micelle after screening in accordance with granularity requirements carries out redrying, does
Dry 160 DEG C of temperature, 25 hours drying times, moisture control less than 2%, that is, prepare the granular titanium silicate of nano aperture；
From lobster shell extraction and deacetylation be 90% 0.5g chitosans be dissolved in 20ml 3% acetic acid solution be made
Chitosan solution, 0.1g titanium silicates are added into chitosan solution, and carrying out ultrasonic wave after well mixed disperses, and adds 2.5g afterwards
Epoxychloropropane and 2.5g OP emulsifying agents, and stir, continuously add alkaline solution, the shell for forming load titanium silicate gathers
Sugared bead, and after being put into alkaline solution by the Chitosan Beads for loading titanium silicate and soak at least 10h, cleaned with distilled water, it
Chitosan Beads are put into sodium hydroxide solution afterwards, and stirred 6 hours at 25 DEG C, then clear is washed with deionized water to load
The Chitosan Beads adsorbent of titanium silicate.
Embodiment 5
Under ice-water bath, in the 500mL flasks equipped with magnetic stirring apparatus, dropping funel and reflux, 40% is added
TEOS ethanol solutions 250g (0.481mol), is uniformly mixed in dropping funel with 30.3mL deionized waters and slowly instills flask
In, after reacting 40 minutes, 50 DEG C are warming up to, by Si/Ti=12, adds 40%TBtOT ethanol solutions 34.1g (4.01 × 10- 2Mol), stir, continuing dropwise addition acid solution is fully hydrolyzed it, after further react 95 minutes, adds 1.25g PEG-
600(2.08×10-3Mol), continue reaction 70 minutes, be cooled to room temperature；Stable sol can be formed by being aged 9 days at 25 DEG C；
Regulation pH value makes colloidal sol be solidified into hydrogel in atmosphere, is filtered through 90 DEG C of deionized water detergent gels untill filtrate pH=7,
Dry 21 hours at a temperature of 145 DEG C, then sieved, the micelle after screening in accordance with granularity requirements carries out redrying, does
Dry 160 DEG C of temperature, 24 hours drying times, moisture control less than 2%, that is, prepare the granular titanium silicate of nano aperture；
From lobster shell extraction and deacetylation be 90% 0.5g chitosans be dissolved in 20ml 3% acetic acid solution be made
Chitosan solution, 0.1g titanium silicates are added into chitosan solution, and carrying out ultrasonic wave after well mixed disperses, and adds 2.0g afterwards
Epoxychloropropane and 2.5g OP emulsifying agents, and stir, continuously add alkaline solution, the shell for forming load titanium silicate gathers
Sugared bead, and after being put into alkaline solution by the Chitosan Beads for loading titanium silicate and soak at least 10h, cleaned with distilled water, it
Chitosan Beads are put into sodium hydroxide solution afterwards, and stirred 6 hours at 25 DEG C, then clear is washed with deionized water to load
The Chitosan Beads adsorbent of titanium silicate.
It can be seen that from embodiment 1~5, inhaled using the high adsorption titanium silicate Chitosan Beads prepared by the inventive method
Attached dose of adsorbance is big, adsorption/desorption speed is fast, regeneration temperature is low, mechanical-physical intensity is high, energy-saving material-saving significant effect, inhales
Attached performance parameter is substantially better than same type adsorbent.
Claims (7)
1. a kind of preparation method of titanium silicate chitosan absorbent, it is characterised in that specifically implement according to following steps：
The preparation of step 1, the spherical titanium silicate in ultra-fine hole：
First allow silicon alkoxide/ethanol solution partial hydrolysis, then heating adds Titanium alkoxides/ethanol solution, allows its complete hydrolysis, then adds
Entering polymeric additive polyethylene glycol makes its polycondensation and is aged colloidal sol is made, and hydrogel is made through oil-free forming technique in colloidal sol, warp
Washing, dry and the spherical titanium silicate of nano aperture is made after sieving；
Step 2, load titanium silicate Chitosan Beads adsorbent preparation：
Titanium silicate made from step 1 is added in chitosan solution, carrying out ultrasonic wave after well mixed disperses, and adds epoxy afterwards
Chloropropane and OP emulsifying agents, and stir, alkaline solution is continuously added, forms the Chitosan Beads of load titanium silicate, and will
The Chitosan Beads of load titanium silicate are put into alkaline solution after immersion, are cleaned with distilled water, are afterwards put into Chitosan Beads
In sodium hydroxide solution, and stirred 4~6 hours at 25 DEG C, then clear is washed with deionized water to the chitosan of load titanium silicate
Bead adsorbent.
A kind of 2. preparation method of titanium silicate chitosan absorbent as claimed in claim 1, it is characterised in that the step 1
In the preparation of colloidal sol specifically comprise the following steps：It is 20%~40% to instill mass fraction into deionized water under ice-water bath
Silicon alkoxide/ethanol solution in, after reacting 30min~45min, be warming up to 40 DEG C~60 DEG C, add mass fraction be 20%~
40% Titanium alkoxides/ethanol solution, is stirred, and continuing dropwise addition acid solution is fully hydrolyzed it, reacts 70min~100min
Afterwards, the polyethylene glycol for accounting for silicon alkoxide and Titanium alkoxides total moles fraction 0.3%~0.6% is added, continues to react 50min~70min
Afterwards, ageing 5d~10d can form stable sol at room temperature.
A kind of 3. preparation method of titanium silicate chitosan absorbent as claimed in claim 2, it is characterised in that the silicon alkoxide
Mol ratio with Titanium alkoxides is 8~20.
A kind of 4. preparation method of titanium silicate chitosan absorbent as claimed in claim 1, it is characterised in that the nano-pore
The preparation of the spherical titanium silicate in footpath specifically comprises the following steps：Using oil-free forming technique, regulation pH value makes colloidal sol in atmosphere
Hydrogel is solidified into, it is scrubbed, 17h~21h is dried at a temperature of 120 DEG C~145 DEG C, is then sieved, and by after screening
Redrying, 130 DEG C~160 DEG C, drying time 21h~25h of drying temperature, moisture control are carried out in accordance with the micelle of granularity requirements
Below 2%, that is, prepare the spherical titanium silicate of nano aperture.
A kind of 5. preparation method of titanium silicate chitosan absorbent as claimed in claim 1, it is characterised in that the step 2
The mass ratio of middle titanium silicate and chitosan is 1：3~5.
A kind of 6. preparation method of titanium silicate chitosan absorbent as claimed in claim 1, it is characterised in that the step 2
Middle chitosan mass is 1 with epoxychloropropane volume ratio：3~5g/ml, added chitosan mass are 1 with OP emulsifying agents volume ratio：
2~3g/ml.
A kind of 7. preparation method of titanium silicate chitosan absorbent as claimed in claim 1, it is characterised in that the step 2
The middle Chitosan Beads for loading titanium silicate are put into alkaline solution soaks at least 10h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1387942A (en) * | 2002-01-14 | 2003-01-01 | 华南理工大学 | Prepn and application of titanium silicate adsorbent with high adsorption performance |
| CN102872832A (en) * | 2012-09-28 | 2013-01-16 | 河海大学 | Preparation method of titanium dioxide loaded chitosan molecular imprinting adsorbent |
| WO2015047991A1 (en) * | 2013-09-24 | 2015-04-02 | Virginia Commonwealth University | Impregnation of oxygen carrier compounds into carrier materials providing compositions and methods for the treatment of wounds and burns |
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Application publication date: 20180109 |