CN109126745A - A kind of recyclable super-hydrophobic powder and preparation method for water-oil separating - Google Patents

A kind of recyclable super-hydrophobic powder and preparation method for water-oil separating Download PDF

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CN109126745A
CN109126745A CN201811134888.2A CN201811134888A CN109126745A CN 109126745 A CN109126745 A CN 109126745A CN 201811134888 A CN201811134888 A CN 201811134888A CN 109126745 A CN109126745 A CN 109126745A
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蔡露
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Chengdu Qiqi Decimal Technology Co Ltd
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    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract

The invention belongs to the technical fields of water-oil separating, provide a kind of recyclable super-hydrophobic powder and preparation method for water-oil separating.This method elder generation in-situ hydrolysis prepares the coated magnetic MFe of nanoscale rough degree, micron-level particle size2O4SiO2Then powder forms one layer of polymethyl methacrylate film on powder surface by emulsifier-free emulsion polymerization, then uses 1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane is surface modified, and Ke Xunhuanliyong super-hydrophobic powder is made.Be compared with the traditional method, super-hydrophobic powder prepared by the present invention, not only have good ultra-hydrophobicity, it is high-efficient for being separated when water-oil separating, and using external magnetic field control composite powder movement with separate, realization recycles.

Description

A kind of recyclable super-hydrophobic powder and preparation method for water-oil separating
Technical field
The invention belongs to the technical field of water-oil separating, provide a kind of for the recyclable super thin of water-oil separating Pigment end and preparation method.
Background technique
In material filtering separation process, oil water mixture is common separation object.Especially in recent years, frequently occur Crude oil and organic matter leakage, cause significant damage to environment and ecology.For leaking into the crude oil and other organic matters of water body, The useful microorganism decomposition of traditional processing method is adsorbed with straw, hair, active carbon etc., or with dispersing agent organic matters such as oil Dispersion etc..The research and application of novel oily water separation technique and material, it has also become more and more important important subject.
The conventional method of water-oil separating has significant limitation, and there is an urgent need to a kind of convenience and high-efficiencies, environment amenable side Method realizes the separation of crude oil and water and the separation of organic matter and water, and the interface performance of material is utilized to carry out the technology of water-oil separating It attracts attention, is mainly divided to two kinds, one is super-hydrophobic super-oleophylic material, for material while repelling water strongly, oil has very it Good wellability;One is underwater superoleophobic surfaces, solid using water-oil-three phase boundary property, material be it is hydrophilic, in water Lower repulsion oil, adhesiveness very little of the oil on material.It is wherein commonly super hydrophobic material.
For super hydrophobic material while water can not soak, oil has good wellability to it, and underwater superoleophobic material has Different materials can be made using their this unique interfacial properties in very strong hydrophily and the very low adhesiveness to oil To realize water-oil separating, thus in fields such as anti-ice, drag reduction and water-oil separatings, crude oil leakage event takes place frequently so that super-hydrophobic material Application of the material in water-oil separating receives significant attention, and bionical interface water-oil separating material is with high oil absorption ability and fast The performance of oil product is recycled, research is rapidly developed, wherein powder specific surface area with higher, by powder super-hydrophobicization Afterwards, a large amount of oil can be adsorbed, excellent water-oil separating material is become, and improve circulation benefit of the super-hydrophobic powder in water-oil separating With becoming current main research.
Chinese invention patent application number 201410225058.6 discloses a kind of preparation method of super-hydrophobic powder comprising Following steps: (1) contain SiO2The preparation of suspension;(2) SiO2The preparation of nanoparticle;(3) it the preparation of super-hydrophobic powder: will walk Suddenly (2) resulting SiO2Nanoparticle, silane coupling agent are added in organic solvent, wherein SiO2Nanoparticle and silane coupling agent Mass volume ratio be 0.3-0.5g/10mL, be stirred to react 15 ~ 20h at 40 ~ 50 DEG C after being sufficiently mixed, obtain suspension, then Resulting suspension is stood into 12 ~ 30h, supernatant liquid is removed, lower sediment thing is dried to obtain super-hydrophobic powder.The invention system Standby super-hydrophobic powder property is good, has broad prospect of application in fields such as water-oil separating, automatically cleanings.But the super-hydrophobic powder It is difficult to effective recycling.
Chinese invention patent application number 201710286873.7 disclose it is a kind of based on flower-shaped iron content manganese dioxide can be same When for lotion separation and Dye Adsorption super-hydrophobic powder preparation method.This includes the system of flower-shaped iron content manganese dioxide Standby, low-surface-energy modification, super-hydrophobic powder is to the processing of lotion and dyestuff.The super-hydrophobic powder has good super thin Water/super-oleophilic energy is all larger than 150 ° to the contact angle of water, and roll angle is less than 10 °, and the contact angle to oil is about 0 °, Neng Gouyong In oil-in-water emulsion point and toxic water-soluble dye absorption.It is not only suitable for work oily waste water and toxic dye polluted-water Processing, while fields such as preparation for the industrial pipeline transport, metal mesh for oil-water separation being also applied for.Defect existing for the invention It is that super-hydrophobic powder obtained efficiently separates recycling, cannot achieve and recycle.
In conclusion the existing super-hydrophobic powder for water-oil separating, there is powder to be difficult to from hot separation and recycle The defect utilized, therefore a kind of super-hydrophobic powder of recyclable water-oil separating is developed, it has great significance.
Summary of the invention
As it can be seen that being used for the super-hydrophobic powder of water-oil separating in the prior art, there is powder to be difficult to from hot separation and recycle The shortcomings that utilization.In response to this, the present invention propose a kind of recyclable super-hydrophobic powder for water-oil separating and Preparation method, not only oil-water separation is good, and can realize and recycle.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating, the tool of the super-hydrophobic powder preparation Steps are as follows for body:
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8 ~ 9, and reaction is hydrolyzed in stirring, by obtained colloidal sol into Row centrifuge separation, is washed, and dry using dehydrated alcohol and deionized water, and nanoscale rough degree, micron-level particle size is made Coated magnetic MFe2O4SiO2Powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;
(3) composite powder made from step (2) is soaked in the 1H, 1H, 2H that mass concentration is 0.2 ~ 0.5%, 2H- perfluoro decyl It in the hexane solution of trichlorosilane, is then washed using dehydrated alcohol and deionized water, re-dry is made for water-oil separating Recyclable super-hydrophobic powder.
Preferably, in step (1) described hydrolysis reaction system, 15 ~ 20 parts by weight of ethyl orthosilicate, deionized water 30 ~ 40 Parts by weight, 30 ~ 50 parts by weight of dehydrated alcohol, magnetic Nano MFe2O45 ~ 10 parts by weight of powder.
Preferably, the MFe2O4Powder is CoFe2O4Powder, NdFe2O4Powder, CeFe2O4Powder, LaFe2O4Powder, NiFe2O4One of powder.
Preferably, the time of step (1) described hydrolysis is 3 ~ 5h, and mixing speed is 60 ~ 90r/min.
Preferably, the revolving speed of step (1) described centrifuge separation is 600 ~ 800r/min, and the time is 20 ~ 30min.
Preferably, in step (2) described emulsion polymerization systems, coated magnetic MFe2O4SiO215 ~ 20 parts by weight of powder, 1 ~ 2 parts by weight of initiator, 3 ~ 5 parts by weight of methyl methacrylate, 73 ~ 81 parts by weight of deionized water.
Preferably, step (2) initiator is ammonium persulfate, potassium peroxydisulfate, methyl ethyl ketone peroxide, cyclohexanone peroxide One of.
Preferably, the mixing speed of step (2) described emulsion polymerization is 40 ~ 80r/min, and the reaction time is 3 ~ 4h.
Preferably, the temperature of step (3) described immersion is 40 ~ 60 DEG C, and the time is 3 ~ 5h.
The present invention hydrolyzes preparation SiO under aqueous ammonia conditions2Powder is dispersed since surfactant not being added, is generated Nano-meter SiO_22Micelle spontaneous can agglomerate into micron-sized particle, and keep nanoscale roughness, this special structure The contact angle of material and water can be increased.Further, a strata methyl is formed on composite powder surface by emulsifier-free emulsion polymerization Methylacrylate Film, then 1H, 1H, 2H are used, 2H- perfluoro decyl trichlorosilane carries out surface chemical modification, due to poly- methyl Methyl acrylate surface polar group rich in can make the silane with fluoro-containing group be easier to modify the table in composite powder Face, to significantly improve the hydrophobic performance of powder, the contact angle of powder and water is significantly increased.
The present invention is in preparation SiO2When powder, by magnetic Nano MFe2O4Powder is added in hydrolyzation system, generates in situ SiO2During micelle, make magnetic Nano MFe2O4Powder is embedded in SiO2In the coarse structure of powder, in water-oil separating, benefit With external magnetic field control composite powder movement with separate, can the oil in water be separated and be conveyed in water easily and isolated Oil, to be difficult to realize powder adsorption material from hot separation after solving the problems, such as super-hydrophobic dusty material absorption oil product Material recycles.
The present invention also provides what a kind of above-mentioned preparation method was prepared to surpass for the recyclable of water-oil separating Drainage powder.The super-hydrophobic powder is the coated magnetic that nanoscale rough degree, micron-level particle size are prepared with first in-situ hydrolysis MFe2O4SiO2Then powder forms one layer of polymethyl methacrylate film on powder surface by emulsifier-free emulsion polymerization, then Using 1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane is surface modified and is made.
It is and existing the present invention provides a kind of recyclable super-hydrophobic powder and preparation method for water-oil separating Technology is compared, and the feature and excellent effect protruded is:
1. super-hydrophobic powder prepared by the present invention has good ultra-hydrophobicity, high-efficient for separating when water-oil separating.
2. super-hydrophobic powder prepared by the present invention has paramagnetism, in water-oil separating, controlled using external magnetic field multiple Close powder movement with separate, realization recycles.
3. preparation method of the invention, raw materials used to be easy to get, preparation process is simple, with good economic efficiency and environment Benefit.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8.5, reaction is hydrolyzed in stirring, the colloidal sol that will be obtained It is centrifuged, is washed using dehydrated alcohol and deionized water, and dry, nanoscale rough degree, micron order grain is made The coated magnetic MFe of diameter2O4SiO2Powder;MFe2O4Powder is CoFe2O4Powder;The time of hydrolysis is 4h, stirring speed Degree is 70r/min;The revolving speed of centrifuge separation is 680r/min, time 26min;In hydrolysis reaction system, ethyl orthosilicate 17 Parts by weight, 34 parts by weight of deionized water, 42 parts by weight of dehydrated alcohol, magnetic Nano MFe2O47 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Ammonium sulfate;The mixing speed of emulsion polymerization is 65r/min, reaction time 3.5h;In emulsion polymerization systems, coated magnetic MFe2O4SiO217 parts by weight of powder, 1 parts by weight of initiator, 4 parts by weight of methyl methacrylate, 78 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 48 DEG C, time 4h.
Embodiment 2
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8, and reaction is hydrolyzed in stirring, by obtained colloidal sol into Row centrifuge separation, is washed, and dry using dehydrated alcohol and deionized water, and nanoscale rough degree, micron-level particle size is made Coated magnetic MFe2O4SiO2Powder;MFe2O4Powder is NdFe2O4Powder;The time of hydrolysis is 3.5h, stirring speed Degree is 70r/min;The revolving speed of centrifuge separation is 650r/min, time 28min;In hydrolysis reaction system, ethyl orthosilicate 16 Parts by weight, 33 parts by weight of deionized water, 45 parts by weight of dehydrated alcohol, magnetic Nano MFe2O46 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Potassium sulfate;The mixing speed of emulsion polymerization is 50r/min, reaction time 4h;In emulsion polymerization systems, coated magnetic MFe2O4 SiO216 parts by weight of powder, 1 parts by weight of initiator, 4 parts by weight of methyl methacrylate, 79 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 45 DEG C, time 4.5h.
Embodiment 3
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 9, and reaction is hydrolyzed in stirring, by obtained colloidal sol into Row centrifuge separation, is washed, and dry using dehydrated alcohol and deionized water, and nanoscale rough degree, micron-level particle size is made Coated magnetic MFe2O4SiO2Powder;MFe2O4Powder is CeFe2O4Powder;The time of hydrolysis is 4.5h, stirring speed Degree is 80r/min;The revolving speed of centrifuge separation is 760r/min, time 22min;In hydrolysis reaction system, ethyl orthosilicate 19 Parts by weight, 37 parts by weight of deionized water, 35 parts by weight of dehydrated alcohol, magnetic Nano MFe2O49 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Methyl Ethyl Ketone Oxidation;The mixing speed of emulsion polymerization is 70r/min, reaction time 3h;In emulsion polymerization systems, coated magnetic MFe2O4SiO219 parts by weight of powder, 2 parts by weight of initiator, 4 parts by weight of methyl methacrylate, 75 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 55 DEG C, time 3.5h.
Embodiment 4
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8, and reaction is hydrolyzed in stirring, by obtained colloidal sol into Row centrifuge separation, is washed, and dry using dehydrated alcohol and deionized water, and nanoscale rough degree, micron-level particle size is made Coated magnetic MFe2O4SiO2Powder;MFe2O4Powder is NiFe2O4Powder;The time of hydrolysis is 5h, mixing speed For 60r/min;The revolving speed of centrifuge separation is 600r/min, time 30min;In hydrolysis reaction system, 15 weight of ethyl orthosilicate Measure part, 30 parts by weight of deionized water, 50 parts by weight of dehydrated alcohol, magnetic Nano MFe2O45 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Peroxyester;The mixing speed of emulsion polymerization is 40r/min, reaction time 4h;In emulsion polymerization systems, coated magnetic MFe2O4SiO215 parts by weight of powder, 1 parts by weight of initiator, 3 parts by weight of methyl methacrylate, 81 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 40 DEG C, time 5h.
Embodiment 5
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 9, and reaction is hydrolyzed in stirring, by obtained colloidal sol into Row centrifuge separation, is washed, and dry using dehydrated alcohol and deionized water, and nanoscale rough degree, micron-level particle size is made Coated magnetic MFe2O4SiO2Powder;MFe2O4Powder is LaFe2O4Powder;The time of hydrolysis is 3h, mixing speed For 90r/min;The revolving speed of centrifuge separation is 800r/min, time 20min;In hydrolysis reaction system, 20 weight of ethyl orthosilicate Measure part, 40 parts by weight of deionized water, 30 parts by weight of dehydrated alcohol, magnetic Nano MFe2O410 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Ammonium sulfate;The mixing speed of emulsion polymerization is 80r/min, reaction time 3h;In emulsion polymerization systems, coated magnetic MFe2O4 SiO220 parts by weight of powder, 2 parts by weight of initiator, 5 parts by weight of methyl methacrylate, 73 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 60 DEG C, time 3h.
Embodiment 6
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8.5, reaction is hydrolyzed in stirring, the colloidal sol that will be obtained It is centrifuged, is washed using dehydrated alcohol and deionized water, and dry, nanoscale rough degree, micron order grain is made The coated magnetic MFe of diameter2O4SiO2Powder;MFe2O4Powder is CeFe2O4Powder;The time of hydrolysis is 4h, stirring speed Degree is 75r/min;The revolving speed of centrifuge separation is 700r/min, time 25min;In hydrolysis reaction system, ethyl orthosilicate 18 Parts by weight, 35 parts by weight of deionized water, 40 parts by weight of dehydrated alcohol, magnetic Nano MFe2O47 parts by weight of powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;Initiator was Potassium sulfate;The mixing speed of emulsion polymerization is 60r/min, reaction time 3.5h;In emulsion polymerization systems, coated magnetic MFe2O4SiO218 parts by weight of powder, 1 parts by weight of initiator, 4 parts by weight of methyl methacrylate, 77 parts by weight of deionized water;
(3) composite powder made from step (2) is soaked in 1H, 1H, 2H, the hexane solution of 2H- perfluoro decyl trichlorosilane In, it is then washed, re-dry, is made for the recyclable super-hydrophobic of water-oil separating using dehydrated alcohol and deionized water Powder;The temperature of immersion is 50 DEG C, time 4h.
Comparative example 1
In preparation process, not formed polymethyl methacrylate film, but directly by MFe2O4/SiO2Composite powder is soaked in It is surface modified in the hexane solution of 1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane, other preparation conditions and embodiment 6 Unanimously.
Comparative example 2
In preparation process, it is not added with magnetic Nano MFe2O4Powder, other preparation conditions and embodiment 6 are consistent.
Performance test:
(1) water contact angle: taking a certain amount of powder produced by the present invention, carries out water using the penetrant method of Washburn equation design and connects The test of feeler measures 5 calculating average values;
(2) cyclic utilization rate: taking super-hydrophobic powder produced by the present invention, and weighing initial mass is M0, oil-water mixture examination is added Test in sample, to oil water separation process after using externally-applied magnetic field and being collected by filtration, then using being done after EtOH Sonicate cleaning It is dry, weigh mass M after test1, cyclic utilization rate A=(M is calculated according to formula0-M1)/M0×100%;
The data obtained is as shown in table 1.
Table 1:

Claims (10)

1. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating, which is characterized in that described super thin Specific step is as follows for the preparation of pigment end:
(1) ethyl orthosilicate is added in the mixed solution of deionized water and dehydrated alcohol, is stirred evenly, magnetism is then added and receives Rice MFe2O4Powder carries out ultrasonic disperse, adds ammonium hydroxide and adjusts pH value to 8 ~ 9, reaction is hydrolyzed in stirring, the colloidal sol that will be obtained It is centrifuged, is washed using dehydrated alcohol and deionized water, and dry, nanoscale rough degree, micron order grain is made The coated magnetic MFe of diameter2O4SiO2Powder;
(2) by coated magnetic MFe made from step (1)2O4SiO2Powder is scattered in deionized water, is passed through N2Air is excluded, Initiator, then continuous dropwise addition methyl methacrylate monomer are added under stirring, by emulsifier-free emulsion polymerization on powder surface Form one layer of polymethyl methacrylate film, filtering, dry, obtained MFe2O4/SiO2/ PMMA composite powder;
(3) composite powder made from step (2) is soaked in the 1H, 1H, 2H that mass concentration is 0.2 ~ 0.5%, 2H- perfluoro decyl It in the hexane solution of trichlorosilane, is then washed using dehydrated alcohol and deionized water, re-dry is made for water-oil separating Recyclable super-hydrophobic powder.
2. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: in step (1) described hydrolysis reaction system, 15 ~ 20 parts by weight of ethyl orthosilicate, 30 ~ 40 parts by weight of deionized water, 30 ~ 50 parts by weight of dehydrated alcohol, magnetic Nano MFe2O45 ~ 10 parts by weight of powder.
3. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, It is characterized in that: step (1) described MFe2O4Powder is CoFe2O4Powder, NdFe2O4Powder, CeFe2O4Powder, LaFe2O4Powder, NiFe2O4One of powder.
4. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: the time of step (1) described hydrolysis is 3 ~ 5h, and mixing speed is 60 ~ 90r/min.
5. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: the revolving speed of step (1) described centrifuge separation is 600 ~ 800r/min, and the time is 20 ~ 30min.
6. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, It is characterized in that: in step (2) described emulsion polymerization systems, coated magnetic MFe2O4SiO215 ~ 20 parts by weight of powder, initiator 1 ~ 2 parts by weight, 3 ~ 5 parts by weight of methyl methacrylate, 73 ~ 81 parts by weight of deionized water.
7. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: step (2) initiator is ammonium persulfate, potassium peroxydisulfate, methyl ethyl ketone peroxide, one in cyclohexanone peroxide Kind.
8. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: the mixing speed of step (2) described emulsion polymerization is 40 ~ 80r/min, and the reaction time is 3 ~ 4h.
9. a kind of preparation method of the recyclable super-hydrophobic powder for water-oil separating according to claim 1, Be characterized in that: the temperature of step (3) described immersion is 40 ~ 60 DEG C, and the time is 3 ~ 5h.
10. any one of claim 1 ~ 9 preparation method is prepared a kind of for the recyclable of water-oil separating Super-hydrophobic powder.
CN201811134888.2A 2018-09-28 2018-09-28 A kind of recyclable super-hydrophobic powder and preparation method for water-oil separating Withdrawn CN109126745A (en)

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CN107486132A (en) * 2017-09-01 2017-12-19 湖南明裕环保科技有限公司 A kind of preparation method of the porous heavy-metal adsorption material of nano ferriferrous oxide
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