CN109232966A - A kind of elastomeric melamine resin oil suction sponge and preparation method - Google Patents
A kind of elastomeric melamine resin oil suction sponge and preparation method Download PDFInfo
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- CN109232966A CN109232966A CN201811185471.9A CN201811185471A CN109232966A CN 109232966 A CN109232966 A CN 109232966A CN 201811185471 A CN201811185471 A CN 201811185471A CN 109232966 A CN109232966 A CN 109232966A
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- C—CHEMISTRY; METALLURGY
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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Abstract
The invention belongs to the technical field of high molecular material, a kind of elastomeric melamine resin oil suction sponge and preparation method are provided.This method first performs etching melamine resin sponge, then in the suspension layers of sponge surface cladding nano-cellulose, slowly heated up dry droplet of the formation containing nano-cellulose, then the dry microballoon for making nano-cellulose form multilayered structure in sponge surface of quick freeze, further deposition trimethylmethoxysilane is surface modified, and elastomeric melamine resin oil suction sponge is made.It is compared with the traditional method, oil suction sponge prepared by the present invention, not only there is good ultra-hydrophobicity, oil absorption efficiency is high, and has good elasticity, remains to maintain ideal deformation-recovery rate and adsorption capacity after recycling.
Description
Technical field
The invention belongs to the technical field of high molecular material, a kind of elastomeric melamine resin oil suction sponge and system are provided
Preparation Method.
Background technique
With the development of industry, polluting caused by the waste water containing greasy dirt, waste liquid, offshore oil leakage etc. can not be ignored,
It does not solve these problems, bigger destruction will be caused to the earth and the mankind.Therefore, oily water separation technique is widely noticed, commonly
Oily water separation technique mainly includes emulsification, absorption, film process, filtering, centrifugation, electrophoresis, flocculation etc..Wherein adsorption technology is because simple
Easy, significant effect, thus it is very popular.
Oil absorption material for water-oil separating as a kind of for handling the functional material of waste oil, for crude oil leakage
Processing, millwork leakage of oil, the processing of effluent oil, processing, the processing of food waste oil of oil etc. in industrial wastewater, tool
It is widely used.Wherein, the research and application of oil suction sponge are more and more.
The oil absorption and water-resistance of the oil absorption materials such as traditional oil suction sponge are weaker, also absorb while oil suction a large amount of
Moisture influences oil absorption efficiency and separating effect.Therefore, the modified technology of hydrophobic oleophilic oil is carried out by pass for oil absorption material surface
Note.In addition, the repeat performance of oil suction sponge is also the important content of its application development.
Chinese invention patent application number 201510121548.6 discloses a kind of high oil absorption sponge for water-oil separating
Preparation method obtains hydrophobically modified the specific steps of which are as follows: first handling on polyurethane sponge skeleton surface with modifying agent
Layer, then by treated, sponge carries out heat-activated processing at a certain temperature, obtains oil suction sponge.The defect of the invention is to inhale
The deformation-recovery rate of oily sponge is not high, and repeat performance is poor.
Chinese invention patent application number 201610351231.6 discloses a kind of system of modified oil suction sponge of hexagonal boron nitride
Preparation Method combines two-dimensional material hexagonal boron nitride and common three-dimensional cavernous structure materials of melamine sponge, step packet
It includes: (1) ultrasonic cleaning of melamine sponge；(2) multilayer h-BN is dispersed, obtains evenly dispersed h-BN nanometer sheet solution；
(3) the melamine sponge cleaned is immersed in evenly dispersed h-BN nanometer sheet solution and is sufficiently infiltrated, obtain six side's nitrogen
Change boron modification oil suction sponge.The defect of the invention is that the hydrophobic performance of gained oil suction sponge needs to be further increased.
In conclusion the oil suction sponge of prior art preparation have deformation-recovery rate after repeated reduce it is obvious,
Adsorption capacity decline is obvious, leads to the disadvantage that service life is short, therefore develops that a kind of deformation-recovery rate is high and absorption property is excellent
Super-hydrophobic oil suction sponge, have great significance.
Summary of the invention
As it can be seen that there is the oil suction sponge of prior art preparation deformation-recovery rate after repeated to reduce obvious, absorption
Ability decline is obvious, leads to the disadvantage that service life is short.In response to this, the present invention proposes a kind of elastomeric melamine resin
Oil suction sponge and preparation method, oil suction sponge obtained not only have good ultra-hydrophobicity, and oil absorption efficiency is high, and has
Good elasticity remains to maintain ideal deformation-recovery rate and adsorption capacity after recycling.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of elastomeric melamine resin oil suction sponge, the specific steps of the high resiliency oil suction sponge preparation are such as
Under:
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, so that the nano-cellulose being adsorbed in the suspension of sponge surface is carried out micro nano structure reconstruct, is formed to sponge surface
It when droplet containing nano-cellulose, is freeze-dried rapidly, nano-cellulose is made to form multilayered structure in sponge surface
The melamine resin sponge that surface is nano-cellulose microballoon is made in microballoon；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Preferably, in step (1) described etching liquid, 20 ~ 30 parts by weight of chrome green, 70 ~ 80 parts by weight of the concentrated sulfuric acid.
Preferably, the time of step (1) described immersion is 10 ~ 20min.
Preferably, the temperature of step (1) described drying is 120 ~ 140 DEG C, and the time is 10 ~ 20min.
Preferably, in step (2) described suspension, 5 ~ 10 parts by weight of nano-cellulose, 90 ~ 95 parts by weight of deionized water.
Preferably, the time of step (2) described immersion is 1 ~ 3h.
Preferably, the heating rate of step (2) described infrared heating is 2 ~ 4 DEG C/min.
Preferably, the temperature of step (2) described freeze-drying is -50 ~ -30 DEG C, and the time is 1 ~ 2h.
The present invention also provides a kind of elastomeric melamine resin oil suction sponges that a kind of above-mentioned preparation method is prepared.
The oil suction sponge is by first performing etching to melamine resin sponge, then in the suspension of sponge surface cladding nano-cellulose
Liquid layer, slowly heated up dry droplet of the formation containing nano-cellulose, and then quick freeze drying makes nano-cellulose in sponge
Surface forms the microballoon of multilayered structure, further deposits trimethylmethoxysilane and is surface modified and is made.
The present invention provides a kind of elastomeric melamine resin oil suction sponge and preparation methods, compared with prior art,
Prominent feature and excellent effect are:
1. melamine resin oil suction sponge prepared by the present invention makes the surface of sponge form the coarse shape of micron order by chemical etching
Then state forms the microballoon of multilayered structure, finally in the table of multi-level coarse structure by the structural remodeling of nano-cellulose
Face is modified using the trimethylmethoxysilane of low-surface-energy, is realized the good ultra-hydrophobicity of melamine resin sponge, is made
It is with excellent oil-water selectivity absorbability and absorptive capacity, oil absorption efficiency height.
2. melamine resin oil suction sponge prepared by the present invention, by the nano-cellulose for introducing multilayered structure in the structure
Microballoon can be absorbed strain using the deformation of nano-cellulose molecule long-chain, increase melamine resin sponge when squeezing fuel-displaced
Elasticity, deformation-recovery rate after extruding significantly improves, and after absorption-extruding repeatedly, remains to maintain ideal deformation recovery
Rate and adsorption capacity, recycling performance is good, long service life.
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) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
16min；Dry temperature is 128 DEG C, time 14min；In etching liquid, 24 parts by weight of chrome green, 76 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 2h；The heating rate of infrared heating is 2 DEG C/min；The temperature of freeze-drying
Degree is -44 DEG C, time 1.5h；In suspension, 7 parts by weight of nano-cellulose, 93 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Embodiment 2
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
12min；Dry temperature is 125 DEG C, time 18min；In etching liquid, 23 parts by weight of chrome green, 77 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 1.5h；The heating rate of infrared heating is 2.5 DEG C/min；Freeze-drying
Temperature be -45 DEG C, time 2h；In suspension, 6 parts by weight of nano-cellulose, 94 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Embodiment 3
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
18min；Dry temperature is 135 DEG C, time 12min；In etching liquid, 28 parts by weight of chrome green, 72 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 2.5h；The heating rate of infrared heating is 3.5 DEG C/min；Freeze-drying
Temperature be -35 DEG C, time 1h；In suspension, 9 parts by weight of nano-cellulose, 91 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Embodiment 4
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
10min；Dry temperature is 120 DEG C, time 20min；In etching liquid, 20 parts by weight of chrome green, 80 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 1h；The heating rate of infrared heating is 2 DEG C/min；The temperature of freeze-drying
Degree is -50 DEG C, time 2h；In suspension, 5 parts by weight of nano-cellulose, 95 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Embodiment 5
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
20min；Dry temperature is 140 DEG C, time 10min；In etching liquid, 30 parts by weight of chrome green, 70 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 3h；The heating rate of infrared heating is 4 DEG C/min；The temperature of freeze-drying
Degree is -30 DEG C, time 1h；In suspension, 10 parts by weight of nano-cellulose, 90 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Embodiment 6
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；The time of immersion is
15min；Dry temperature is 130 DEG C, time 15min；In etching liquid, 25 parts by weight of chrome green, 75 weight of the concentrated sulfuric acid
Part；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, it when sponge surface forms the droplet containing nano-cellulose, is freeze-dried rapidly, it is nano-cellulose that surface, which is made,
The melamine resin sponge of microballoon；The time of immersion is 2h；The heating rate of infrared heating is 3 DEG C/min；The temperature of freeze-drying
Degree is -40 DEG C, time 1.5h；In suspension, 8 parts by weight of nano-cellulose, 92 parts by weight of deionized water；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
Comparative example 1
It in preparation process, does not perform etching, other preparation conditions and embodiment 6 are consistent.
Comparative example 2
In preparation process, unsupported nano-cellulose microballoon, other preparation conditions and embodiment 6 are consistent.
Comparative example 3
In preparation process, trimethylmethoxysilane is not deposited, other preparation conditions and embodiment 6 are consistent.
Performance test:
(1) water contact angle: taking the oil suction sponge produced by the present invention of arbitrary shape, using OCA20 video optics contact angle determination
The test of instrument hydrophobic properties of the surface, test carry out at room temperature, and drop size used is 5 μ L, respectively 5 or more different positions
It sets measurement and calculates average value
(2) deformation-recovery rate: by oil suction sponge produced by the present invention be made side length be 10cm sample, compressional deformation to 70%, to
The volume ratio that sponge sample is tested after recovery, is calculated deformation recovery rate；
(3) diesel oil adsorbance: sample is cut into 2cm × 2cm × 1cm cube, claims its quality；Cuboid sample is packed into iron
It in silk screen, immerses in diesel oil respectively at room temperature, takes out, weighed rapidly after drip 2min at regular intervals, diesel oil is inhaled
Attached amount calculates according to the following formula: diesel oil adsorbance (g/g)=(M2- M1- M0)/M0, in formula: M0For foams original quality；M1For iron
Silk screen quality；M2For foam quality after oil suction；
(4) performance is recycled: will squeeze and be filtered dry after oil suction steel foams saturation, then repeat to test, obtain for the first time with
Deformation-recovery rate and diesel oil adsorbance at 50 times.
The data obtained is as shown in table 1.
Table 1:
Claims (9)
1. a kind of preparation method of elastomeric melamine resin oil suction sponge, which is characterized in that the high resiliency oil suction sponge system
It is standby that specific step is as follows:
(1) chrome green is added in the concentrated sulfuric acid (mass fraction 98.3%) and etching liquid is made, then by melamine resin sponge
It immerses in etching liquid, immersion is taken out after a certain period of time, and it is dry, obtain the melamine resin sponge of surface etch；
(2) nano-cellulose is added in deionized water, ultrasonic disperse forms uniform and stable suspension, then by step (1)
Etching melamine resin sponge obtained is immersed in suspension, and immersion is taken out after a certain period of time, is slowly heated up using infrared ray
It is dry, so that the nano-cellulose being adsorbed in the suspension of sponge surface is carried out micro nano structure reconstruct, is formed to sponge surface
It when droplet containing nano-cellulose, is freeze-dried rapidly, nano-cellulose is made to form multilayered structure in sponge surface
The melamine resin sponge that surface is nano-cellulose microballoon is made in microballoon；
(3) trimethylmethoxysilane is further deposited on by sponge surface made from step (2) as vapour deposition process
Obtain elastomeric melamine resin oil suction sponge.
2. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(1) in the etching liquid, 20 ~ 30 parts by weight of chrome green, 70 ~ 80 parts by weight of the concentrated sulfuric acid.
3. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(1) time of the immersion is 10 ~ 20min.
4. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(1) temperature of the drying is 120 ~ 140 DEG C, and the time is 10 ~ 20min.
5. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(2) in the suspension, 5 ~ 10 parts by weight of nano-cellulose, 90 ~ 95 parts by weight of deionized water.
6. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(2) time of the immersion is 1 ~ 3h.
7. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(2) heating rate of the infrared heating is 2 ~ 4 DEG C/min.
8. a kind of preparation method of elastomeric melamine resin oil suction sponge according to claim 1, it is characterised in that: step
(2) temperature of the freeze-drying is -50 ~ -30 DEG C, and the time is 1 ~ 2h.
9. a kind of elastomeric melamine resin oil suction sponge that any one of claim 1 ~ 8 preparation method is prepared.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628076A (en) * | 2019-10-09 | 2019-12-31 | 西南石油大学 | Simple method for modifying melamine sponge by super-hydrophobicity |
| CN111646541A (en) * | 2020-02-29 | 2020-09-11 | 杭州电子科技大学 | Offshore oil cleaning and recycling device |
| CN113385046A (en) * | 2021-06-24 | 2021-09-14 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
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| CN105399977A (en) * | 2015-12-04 | 2016-03-16 | 武汉工程大学 | Method for preparing reusable oil-absorbing sponge |
| CN105413656A (en) * | 2015-12-03 | 2016-03-23 | 梅庆波 | Preparation method of super-hydrophobic polyurethane sponge/iron oxide composite material used for oil-water separation |
| CN107243327A (en) * | 2017-05-26 | 2017-10-13 | 玉灵华科技有限公司 | Cellulose microsphere for depth-averaged model is prepared and sewage water treatment method |
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| JPS61172561A (en) * | 1985-01-28 | 1986-08-04 | 株式会社神戸製鋼所 | Deodorant |
| CN105413656A (en) * | 2015-12-03 | 2016-03-23 | 梅庆波 | Preparation method of super-hydrophobic polyurethane sponge/iron oxide composite material used for oil-water separation |
| CN105399977A (en) * | 2015-12-04 | 2016-03-16 | 武汉工程大学 | Method for preparing reusable oil-absorbing sponge |
| CN107243327A (en) * | 2017-05-26 | 2017-10-13 | 玉灵华科技有限公司 | Cellulose microsphere for depth-averaged model is prepared and sewage water treatment method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628076A (en) * | 2019-10-09 | 2019-12-31 | 西南石油大学 | Simple method for modifying melamine sponge by super-hydrophobicity |
| CN110628076B (en) * | 2019-10-09 | 2022-01-28 | 西南石油大学 | Simple method for modifying melamine sponge by super-hydrophobicity |
| CN111646541A (en) * | 2020-02-29 | 2020-09-11 | 杭州电子科技大学 | Offshore oil cleaning and recycling device |
| CN113385046A (en) * | 2021-06-24 | 2021-09-14 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
| CN113385046B (en) * | 2021-06-24 | 2022-05-10 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
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| CN109232966B (en) | 2021-01-22 |
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