CN108097216A - A kind of environmental-protection adsorption magnetic microsphere and preparation method thereof - Google Patents

A kind of environmental-protection adsorption magnetic microsphere and preparation method thereof Download PDF

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CN108097216A
CN108097216A CN201711278946.4A CN201711278946A CN108097216A CN 108097216 A CN108097216 A CN 108097216A CN 201711278946 A CN201711278946 A CN 201711278946A CN 108097216 A CN108097216 A CN 108097216A
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金昱轩
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    • 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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    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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

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Abstract

The invention discloses a kind of environmental-protection adsorption magnetic microspheres, it is made of the raw material of following weight parts：β hydroxyalkyl amides 12, four water frerrous chlorides 30 40, ferric chloride (FeCl36H2O) 24 30, dodecyl trimethyl ammonium chloride 0.7 1, casein 23, butyl titanate 41 50, ricinoleic acid 12, nano-carbon powder 10 13, amine reagent 13.The microballoon of the present invention has good magnetic absorption effect, is blended with carbon dust, has good synergistic sorption performance, can be widely applied to air purification.

Description

A kind of environmental-protection adsorption magnetic microsphere and preparation method thereof
Technical field
The invention belongs to microballoon fields, and in particular to a kind of environmental-protection adsorption magnetic microsphere and preparation method thereof.
Background technology
As a kind of organized architecture structure, the hollow nanostructured property that brings many general nano materials and can not obtain Can, there are many new purposes.For the preparation of relatively general nano-particle, the preparation difficulty of hollow nano-material is larger, It is difficult to it is directly obtained with general synthetic technology.The method for preparing hollow nanometer material reported at present mainly have self-assembly method, Template, hydrothermal synthesis method, sol-gel method, jet nozzle reactors method, emulsion interface polymerization and curing method etc..Wherein template Method is when former more effective simple preparation method most directly perceived, is widely used general, generally comprises four steps, 1. template Preparation 2. to template carry out surface modified function 3. existed by various methods with obtaining specific Surface Physical Chemistry performance Template surface deposits Shell Materials, it may be necessary to be post-processed, 4. selectively be etched with the complete shell for obtaining fine and close Mould material is removed, hollow nano-material is made.It can be seen that the step of being typically prepared hollow nano-material is all comparatively laborious, more grind The step of person of studying carefully points out to prepare just because of hollow nano-material is cumbersome, seriously hinders its industrialization and application.Therefore, simplify The preparation process of hollow nano-material has important theory significance and realistic meaning.
For template preparation, mould material desired size narrowly distributing, the business for being easily largely made, having different dimensions Industryization is supplied or can prepared with simple classical way.At present, it is concentrated mainly on monodispersed dioxy using most templates SiClx colloidal sol nano-particle and pipe/polyhenylethylene nano latex particle are also exactly carbosphere, metal nanoparticle and metal oxidation Object particle template.It is typically all the method with the dissolving of suitable solvent or high-temperature calcination to remove template, it is important to remove mould Plate backskin material cannot cave in, therefore dissolve removing template preferably by solvent.Effectively intactly deposited in template surface Shell Materials are most challenged, because nuclear material and shell material often mismatches such as lattice or surface property.This just needs to lead to It crosses and template progress surface modified function is overcome with obtaining specific functionalization group or property, such as power on its surface band Lotus in some cases, can carry out surface-functionalized while template is prepared, and surface band such as is made by one step of combined polymerization The functional polymer template of functional group can so simplify the preparation process of hollow nano-material.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of environmental-protection adsorption magnetic microsphere and its Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of environmental-protection adsorption magnetic microsphere, it is made of the raw material of following weight parts：
Beta-hydroxy alkylamide 1-2, four water frerrous chloride 30-40, ferric chloride (FeCl36H2O) 24-30, trimethyl chlorine Change ammonium 0.7-1, casein 2-3, butyl titanate 41-50, ricinoleic acid 1-2, nano-carbon powder 10-13, amine reagent 1-3.
The preparation method of the environmental-protection adsorption magnetic microsphere, comprises the following steps：
(1) amine reagent is taken, is added in the deionized water of 7-9 times of its weight, stirs evenly, above-mentioned concentration is added dropwise as 10- 13% ammonium hydroxide, stirs evenly, and obtains amine aqueous solution；
(2) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added to the deionized water of 20-30 times of mixture weight In, it stirs evenly, rise temperature is 75-80 DEG C, and above-mentioned amine aqueous solution is added dropwise, when insulated and stirred 1-2 is small, obtains amination magnetic solution；
(3) nano-carbon powder, beta-hydroxy alkylamide mixing are taken, is added in the deionized water of 20-30 times of mixture weight, adds Enter ricinoleic acid, it is 10-20 minutes ultrasonic, obtain carbon dust amide solution；
(4) butyl titanate is taken, is added in the deionized water of 23-30 times of its weight, stirs evenly, be sent to 30-35 DEG C water bath with thermostatic control in, add in above-mentioned amination magnetic solution, when insulated and stirred 3-5 is small, obtain Sol-gel Coated magnetic solution；
(5) above-mentioned carbon dust amide solution, the mixing of Sol-gel Coated magnetic solution are taken, rise temperature is 70-75 DEG C, insulated and stirred When 2-4 is small, precipitation is washed in filtering, when drying 1-2 is small at 60-65 DEG C of vacuum, is cooled to room temperature to get the environmental-protection adsorption Magnetic microsphere.
The amine reagent is ethylenediamine.
Advantages of the present invention：
The present invention, by being hydrolyzed in amine aqueous solution, obtains amination magnetic using four water frerrous chlorides, ferric chloride (FeCl36H2O) as presoma Property solution, then by nano-carbon powder using ricinoleic acid handle, be distributed to afterwards in amide aqueous solution, obtain carbon dust amide solution, Then using butyl titanate as presoma, by being hydrolyzed in amination magnetic solution, Sol-gel Coated magnetic solution is obtained, finally will It is blended with carbon dust amide solution, passes through amine and the blending reaction of ricinoleic acid so that carbon dust has compatible well with colloidal sol Property, so as to the microballoon stablized, microballoon of the invention has good magnetic absorption effect, is blended with carbon dust, has very Good synergistic sorption performance, can be widely applied to air purification.
Specific embodiment
Embodiment 1
A kind of environmental-protection adsorption magnetic microsphere, it is made of the raw material of following weight parts：
Beta-hydroxy alkylamide 1, four water frerrous chlorides 30, ferric chloride (FeCl36H2O) 24, dodecyl trimethyl ammonium chloride 0.7, Casein 2, butyl titanate 41, ricinoleic acid 1, nano-carbon powder 10, amine reagent 1-3.
The preparation method of the environmental-protection adsorption magnetic microsphere, comprises the following steps：
(1) amine reagent is taken, is added in the deionized water of 7 times of its weight, stirs evenly, it is 10% that above-mentioned concentration, which is added dropwise, Ammonium hydroxide stirs evenly, and obtains amine aqueous solution；
(2) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 20 times of mixture weight, It stirs evenly, rise temperature is 75 DEG C, and above-mentioned amine aqueous solution is added dropwise, when insulated and stirred 1 is small, obtains amination magnetic solution；
(3) nano-carbon powder, beta-hydroxy alkylamide mixing are taken, is added in the deionized water of 20 times of mixture weight, adds in Ricinoleic acid, ultrasound 10 minutes, obtains carbon dust amide solution；
(4) butyl titanate is taken, is added in the deionized water of 23 times of its weight, stirs evenly, be sent to 30 DEG C of perseverance In tepidarium, above-mentioned amination magnetic solution is added in, when insulated and stirred 3 is small, obtains Sol-gel Coated magnetic solution；
(5) above-mentioned carbon dust amide solution, the mixing of Sol-gel Coated magnetic solution are taken, rise temperature is 70 DEG C, and insulated and stirred 2 is small When, precipitation is washed in filtering, when drying 1 is small at 60 DEG C of vacuum, is cooled to room temperature to get the environmental-protection adsorption magnetic microsphere.
Embodiment 2
A kind of environmental-protection adsorption magnetic microsphere, it is made of the raw material of following weight parts：
It is beta-hydroxy alkylamide 2, four water frerrous chlorides 40, ferric chloride (FeCl36H2O) 30, dodecyl trimethyl ammonium chloride 1, dry Casein 3, butyl titanate 50, ricinoleic acid 2, nano-carbon powder 13, amine reagent 3.
The preparation method of the environmental-protection adsorption magnetic microsphere, comprises the following steps：
(1) amine reagent is taken, is added in the deionized water of 9 times of its weight, stirs evenly, it is 13% that above-mentioned concentration, which is added dropwise, Ammonium hydroxide stirs evenly, and obtains amine aqueous solution；
(2) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 30 times of mixture weight, It stirs evenly, rise temperature is 80 DEG C, and above-mentioned amine aqueous solution is added dropwise, when insulated and stirred 2 is small, obtains amination magnetic solution；
(3) nano-carbon powder, beta-hydroxy alkylamide mixing are taken, is added in the deionized water of 30 times of mixture weight, adds in Ricinoleic acid, ultrasound 20 minutes, obtains carbon dust amide solution；
(4) butyl titanate is taken, is added in the deionized water of 30 times of its weight, stirs evenly, be sent to 35 DEG C of perseverance In tepidarium, above-mentioned amination magnetic solution is added in, when insulated and stirred 5 is small, obtains Sol-gel Coated magnetic solution；
(5) above-mentioned carbon dust amide solution, the mixing of Sol-gel Coated magnetic solution are taken, rise temperature is 75 DEG C, and insulated and stirred 4 is small When, precipitation is washed in filtering, when drying 2 is small at 65 DEG C of vacuum, is cooled to room temperature to get the environmental-protection adsorption magnetic microsphere.
Performance test：
Formaldehyde is passed through in 3 Laboratory Modules so that the concentration of formaldehyde of 3 Laboratory Modules is 3.0 milligrams/cubic metre respectively；It incite somebody to action this 1 environmental-protection adsorption magnetic microsphere of inventive embodiments, 2 environmental-protection adsorption magnetic microsphere of embodiment, commercially available carbon dust are respectively as 3 Laboratory Modules In, the size of Laboratory Module is 30 cubic metres, 1 micro-porous adsorption type automotive interior material of embodiment, 2 micro-porous adsorption type vapour of embodiment Interior exterior material, the dosage of commercially available carbon dust are 1kg；After when Laboratory Module sealing 24 is small, the formaldehyde removing rate of each Laboratory Module is surveyed；
The formaldehyde removing rate for the Laboratory Module that 1 porous zeolite material for air purification of embodiment is placed：95.7%；
The formaldehyde removing rate for the Laboratory Module that 2 porous zeolite material for air purification of embodiment is placed：96.1%；
The formaldehyde removing rate for the Laboratory Module that commercially available carbon dust is placed：59.4%.

Claims (3)

1. a kind of environmental-protection adsorption magnetic microsphere, which is characterized in that it is made of the raw material of following weight parts：
Beta-hydroxy alkylamide 1-2, four water frerrous chloride 30-40, ferric chloride (FeCl36H2O) 24-30, dodecyl trimethyl ammonium chloride 0.7-1, casein 2-3, butyl titanate 41-50, ricinoleic acid 1-2, nano-carbon powder 10-13, amine reagent 1-3.
2. a kind of preparation method of environmental-protection adsorption magnetic microsphere as described in claim 1, which is characterized in that including following step Suddenly：
(1) amine reagent is taken, is added in the deionized water of 7-9 times of its weight, stirs evenly, above-mentioned concentration is added dropwise as 10-13% Ammonium hydroxide, stir evenly, obtain amine aqueous solution；
(2) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 20-30 times of mixture weight, stirs It mixes uniformly, rise temperature is 75-80 DEG C, and above-mentioned amine aqueous solution is added dropwise, when insulated and stirred 1-2 is small, obtains amination magnetic solution；
(3) nano-carbon powder, beta-hydroxy alkylamide mixing are taken, is added in the deionized water of 20-30 times of mixture weight, adds in castor Sesame oil acid, it is 10-20 minutes ultrasonic, obtain carbon dust amide solution；
(4) butyl titanate is taken, is added in the deionized water of 23-30 times of its weight, stirs evenly, be sent to 30-35 DEG C In water bath with thermostatic control, above-mentioned amination magnetic solution is added in, when insulated and stirred 3-5 is small, obtains Sol-gel Coated magnetic solution；
(5) above-mentioned carbon dust amide solution, the mixing of Sol-gel Coated magnetic solution are taken, rise temperature is 70-75 DEG C, insulated and stirred 2-4 Hour, precipitation is washed in filtering, when drying 1-2 is small at 60-65 DEG C of vacuum, is cooled to room temperature magnetic to get the environmental-protection adsorption Microballoon.
3. a kind of environmental-protection adsorption magnetic microsphere according to claim 1, which is characterized in that the amine reagent is ethylenediamine.
CN201711278946.4A 2017-12-06 2017-12-06 A kind of environmental-protection adsorption magnetic microsphere and preparation method thereof Pending CN108097216A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110090625A (en) * 2018-05-15 2019-08-06 赖凯旋 A kind of photocatalysis air-cleaning material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104801262A (en) * 2014-01-27 2015-07-29 中国科学院上海高等研究院 Preparation method and application of magnetic composite uranium adsorbent
CN106215937A (en) * 2016-07-04 2016-12-14 江苏大学 A kind of based on the loaded mesoporous TiO of magnetic carbon material2the preparation method and its usage of composite photo-catalyst
CN107321324A (en) * 2017-09-05 2017-11-07 霍邱金木鱼农业科技有限公司 A kind of dye discoloration magnetic adsorptive material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104801262A (en) * 2014-01-27 2015-07-29 中国科学院上海高等研究院 Preparation method and application of magnetic composite uranium adsorbent
CN106215937A (en) * 2016-07-04 2016-12-14 江苏大学 A kind of based on the loaded mesoporous TiO of magnetic carbon material2the preparation method and its usage of composite photo-catalyst
CN107321324A (en) * 2017-09-05 2017-11-07 霍邱金木鱼农业科技有限公司 A kind of dye discoloration magnetic adsorptive material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110090625A (en) * 2018-05-15 2019-08-06 赖凯旋 A kind of photocatalysis air-cleaning material and preparation method thereof

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Application publication date: 20180601