CN105906909A - High-density polyethylene oil-water separation material and preparation method thereof - Google Patents
High-density polyethylene oil-water separation material and preparation method thereof Download PDFInfo
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- CN105906909A CN105906909A CN201610330833.3A CN201610330833A CN105906909A CN 105906909 A CN105906909 A CN 105906909A CN 201610330833 A CN201610330833 A CN 201610330833A CN 105906909 A CN105906909 A CN 105906909A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
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Abstract
The invention discloses a high-density polyethylene oil-water separation material and a preparation method thereof. The method comprises the following steps: with polyethylene oxide and high-density polyethylene as raw materials, performing melt extrusion with an extruder, and coiling and collecting with a coiling machine; leaching the collected sample with deionized water to remove the polyethylene oxide; and performing freeze drying treatment with a refrigerator and a freeze dryer to obtain the high-density polyethylene oil-water separation material. The method has the advantages of simple technology, short time, no chemicals or consequent environmental pollution and low cost. The high-density polyethylene oil-water separation material prepared by the method comprises a structure of high-density polyethylene continuous filament, and the structure has pores with diameter of several microns to over ten microns, shows a porous oriented fiber-like structure and realizes a relatively good adsorption effect on oil and organic reagent; and the sample has continuous length, is soft and can be woven into large-area oil-water separation fabric, thereby providing an effective solution for controlling the offshore oil leakage and purifying domestic sewage.
Description
Technical field
The invention belongs to new material processing preparation field, relate to the preparation method of a kind of three-dimensional porous oil-water separation material, particularly relate to a kind of high density polyethylene (HDPE) oil-water separation material and preparation method thereof.
Background technology
Coming in administer Crude Oil at Sea leakage and purification oil-containing sanitary sewage is faced with increasing challenge, current administering method is probably divided into following several: utilizes the oil on the material recovery water surface of hydrophobic oleophilic oil character, utilize dispersant by oil mixing with water to promote that its natural degradation, directly burning are to remove oil slick.The method that ordinary priority considers is to use to have the material of hydrophobic oleophilic oil character to reclaim slick, because so can dealing carefully with oil slick, will not producing secondary pollution again.The material of these currently used hydrophobic oleophilic oil can be divided into drainage powder material, hydrophobic-film materials and hydrophobic three-dimensional porous material.
When hydrophobic three-dimensional porous material is applied to oil water separation process, can provide the space of storage oil product owing to having abundant gap structure, the oil absorption making material is relatively big, has significant advantage in actual applications.Super-hydrophobic concept is incorporated in the application of oil-water separation by 2004 Nian Jiang thunder seminars first, and is successfully prepared the metal grill of super-hydrophobic super-oleophylic；Under the conditions of Sun Li great waves seminar utilizes the method for chemical reaction that the aqueous dispersions of graphite oxide is placed in 180 DEG C, thermal reduction forms Graphene hydrogel after 24 hours, then hydrogel is obtained graphene aerogel through lyophilization, the aeroge prepared has loose structure and hydrophobic--oil-wet behavior, the mechanical strength of this three-dimensional porous hydrophobic material is poor, three-dimensional framework can not deform upon or be easier to crushed destruction, and to carry out the suitability in the complex environment that water is separating of oil relatively low actual；Tsing-Hua University Wu De sea seminar is prepared for the fast package material of CNT of three-dimensional porous sponge shape by chemical vapour deposition technique, CNT sponge has superhydrophobic characteristic, abundant gap structure and ultralight density make material have stronger oil absorption, the amount that can absorb organic solvent or oil product is about 80 ~ 180 times of own wt, but preparation method is complicated, cost high；And the electrospinning process that prior art is conventional, use the method need when preparing oil-water separation material organic solvent addition, be detrimental to health, environmental pollution, and preparation time is long, reduces production efficiency and is unfavorable for that large-scale industrial production is applied.Said method has all prepared three-dimensional porous oil-water separation material, but these preparation methoies have, and preparation process is complicated, use chemical reagent to cause environmental pollution, be difficult to the feature of large-scale production and application, is unfavorable for instructing industrialized production.
High density polyethylene (HDPE) (HDPE) is one of most widely used general-purpose plastics, and it is cheap and easy to get, stable performance, technology of preparing are ripe, and high density polyethylene (HDPE) belongs to environmental-protecting material, and heating reaches fusing point and gets final product recycling.High density polyethylene (HDPE) itself has the character of hydrophobic oleophilic oil, after being processed into three-dimensional porous material, can more effectively carry out oil-water separation, compared with other water oil separation materials (such as CNT sponge, graphene aerogel etc.), it is easily processed into type, preparation cost is low, can be used repeatedly, be conducive to large-scale continuous production, be suitable to industrial applications.But at present high density polyethylene (HDPE) is processed as oil-water separation material and needs complex preparation method and equipment, relatively costly, it is unfavorable for large-scale production and application.
Summary of the invention
In order to solve the problems referred to above, the invention provides the preparation method of a kind of high density polyethylene (HDPE) oil-water separation material, the method technological process is simple, easy and simple to handle, it is not necessary to the addition of chemicals, environmental friendliness, and production cost is low, can apply with large-scale continuous production.
The oil-water separation material using the inventive method to prepare includes high density polyethylene (HDPE) continuous tow structure, and this fibre bundle presents porous orientation filamentary structure, can be compiled into large-area oil-water separation fabric, have efficient oil-water separation.
The present invention is achieved by the following technical solutions
The preparation method of a kind of high density polyethylene (HDPE) oil-water separation material, comprises the following steps:
(1) poly(ethylene oxide) powder and deionized water are mixed to form pasty state, then mixture are placed in baking oven and dry until its quality no longer changes, after being cooled to room temperature, be broken for poly(ethylene oxide) pellet；
(2) poly(ethylene oxide) pellet step (1) obtained and pellets of high density polyethylene join to melt extrude in extruder and obtain continuous rope form material strip；Wherein the mass fraction shared by poly(ethylene oxide) is 10 ~ 60%；
(3) continuous rope form material strip step (2) melt extruded, is collected under tensionless winkler foundation state with coiling machine, and the continuous rope form material strip collected is cut into the continuous material strip of segment；
(4) segment continuous rope form material step (3) obtained utilizes deionized water to carry out supersound process at normal temperatures, and leaching removes water miscible poly(ethylene oxide), until the quality of the continuous material strip of segment no longer changes；
(5) the continuous material strip of segment after the leaching that will obtain in step (4) is placed in refrigerator freezing, and freezing is dried process in freezer dryer and obtains high density polyethylene (HDPE) oil-water separation material after completing, detect.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, the molecular weight of described poly(ethylene oxide) powder is 100000 ~ 200000, for polyethylene glycol oxide PEO.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, when the poly(ethylene oxide) powder described in step (1) mixes with deionized water, the mass fraction of poly(ethylene oxide) is 40 ~ 50%.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, the baking temperature of the oven drying described in step (1) is 30 ~ 40 DEG C, drying time is 2 ~ 3 days；The particle diameter of the described broken poly(ethylene oxide) pellet obtained is 0.8 ~ 1.2mm.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, the mass fraction shared by step (2) described poly(ethylene oxide) is 50%.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, described high density polyethylene (HDPE) oil-water separation material is high density polyethylene (HDPE) continuous tow, and described high density polyethylene (HDPE) continuous tow has a diameter of 1 μm hole to 20 μm.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, the extruder described in step (2) is Minitype twin-screw extrusion machine；When described raw material melt extrudes in an extruder, the temperature melt extruded is 140 ~ 160 DEG C, the rotating speed of extruder screw is 8 ~ 12rpm；Step (3) described coiling machine is when being collected, and the speed of collecting of coiling machine is 20 ± 2cm/min.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, step (5) described material strip temperature of freezing in refrigerator is-20 ~-15 DEG C, cooling time is 2 ~ 5 hours；Temperature when being dried in fridge is-85 ~-80 DEG C, vacuum is 0 ~ 1pa, and the cryodesiccated time is 48 ~ 72 hours.
The preparation method of described high density polyethylene (HDPE) oil-water separation material, the application in oil-water separation of the described high density polyethylene (HDPE) oil-water separation material.
A kind of high density polyethylene (HDPE) oil-water separation material, described high density polyethylene (HDPE) oil-water separation material is prepared by said method.
Poly(ethylene oxide) and high density polyethylene (HDPE) with different mass ratio mixing extrusion moldings, are then removed poly(ethylene oxide) by deionized water leaching by the present invention, form the oil-water separation material of different structure.When the mass ratio of poly(ethylene oxide) Yu high density polyethylene (HDPE) is 1:1, form the hdpe fiber bundle being made up of fento.The method utilizing method for processing forming extrusion molding and leaching carrys out processing and forming high density polyethylene (HDPE) oil-water separation material, there is process operation simplicity, low cost, the raw material used does not contains chemicals, environmentally safe, low cost, product is soft, length is continuous, and can be mass-produced the advantages such as application.The material prepared has preferable oil-water separation.
Compared with prior art, the present invention has a following positive beneficial effect:
(1) present invention utilizes the method for extrusion molding and leaching to be prepared for high density polyethylene (HDPE) oil-water separation material, solves and is difficult to serialization, scale, the problem of low-cost production porous oil-water separation material in existing preparation method；
(2) preparation method utilizing the present invention during preparing high density polyethylene (HDPE) oil-water separation material raw materials used cheap and easy to get, there is no an addition of chemicals, pollution-free and greatly reduce production cost, course of processing safety and environmental protection；
(3) can prepare the high density polyethylene (HDPE) continuous tow being made up of fento for oil-water separation by the preparation method of the present invention, the size of its hole is micro-meter scale, and this material presents porous orientation filamentary structure, has higher adsorption efficiency；This polyethylene continuous tow length is continuous, soft, can be woven into large-area oil-water separation fabric, provides effective solution for administering Crude Oil at Sea leakage and purification oil-containing sanitary sewage；
(4) the hdpe fiber bundle that the present invention utilizes extruding forming method to prepare is long for service life in oil-water separation is applied, use after this material oil suction after centrifugal treating, oil-water separation can be reused for, still there is good oil absorbing effect, repetitive cycling uses and is maintained to good oil absorbing effect 100 times, not only greatly reduce the cost of oil-water separation, also achieve the collection recycling of waste oil, there are higher economic results in society.
Accompanying drawing explanation
Fig. 1 is the storage modulus situation of change with angular frequency of the different samples that raw material poly(ethylene oxide) is prepared when different quality proportioning from high density polyethylene (HDPE)；
Fig. 2 is the macroscopic form figure that mass ratio is high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A prepared during 1:1 of poly(ethylene oxide) and high density polyethylene (HDPE), macrograph before wherein Fig. 2 a is leaching poly(ethylene oxide), 2b is the macroscopic form figure after leaching poly(ethylene oxide)；
Fig. 3 is the microscopic pattern figure that mass ratio is high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A prepared during 1:1 of poly(ethylene oxide) and high density polyethylene (HDPE), wherein Fig. 3 a is the high density polyethylene (HDPE) continuous tow sample A scanning electron microscope shape appearance figure along extrusion direction, and Fig. 3 b is the partial enlarged drawing of Fig. 3 a；Fig. 3 c is the ultramicroscope shape appearance figure that high density polyethylene (HDPE) continuous tow A is perpendicular to extrude direction, and Fig. 3 d is the partial enlarged drawing of Fig. 3 c；
Fig. 4 is the macroscopic form figure of the high density polyethylene (HDPE) oil-water separation material B prepared during the mass ratio 1:9 of poly(ethylene oxide) and high density polyethylene (HDPE), and the macrograph before wherein Fig. 4 a is leaching oxirane, Fig. 4 b is the macroscopic form figure after leaching oxirane；
Fig. 5 poly(ethylene oxide) and the microscopic pattern figure that mass ratio is the high density polyethylene (HDPE) oil-water separation material B prepared during 1:9 of high density polyethylene (HDPE), wherein Fig. 5 a is the high density polyethylene (HDPE) oil-water separation material B scanning electron microscope shape appearance figure along extrusion direction, and Fig. 5 b is the enlarged drawing of Fig. 5 a；Fig. 5 c is the scanning electron microscope shape appearance figure that high density polyethylene (HDPE) oil-water separation material B is perpendicular to extrude direction, and Fig. 5 d is the enlarged drawing of Fig. 5 c；
Fig. 6 is that the mass ratio of raw material poly(ethylene oxide) and high density polyethylene (HDPE) is respectively 1:9, the product high density polyethylene (HDPE) oil-water separation material prepared when 1:1,1.5:1 structural representation before and after leaching；
Fig. 7 is raw material poly(ethylene oxide) and the mass ratio of high density polyethylene (HDPE) is the continuous material strip on the left of 9:1(beaker) and mass ratio be the continuous material strip on the right side of 1:1(beaker) time the oil suction dynamic contrast figure of high density polyethylene (HDPE) oil-water separation material prepared；
Fig. 8 is raw material poly(ethylene oxide) and the mass ratio of high density polyethylene (HDPE) is that high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A prepared during 1:1 carries out the lab diagram of oil-water separation；
Fig. 9 is that continuous rope form material strip high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A for preparing when being 1:1 with high density polyethylene (HDPE) mass ratio of raw material poly(ethylene oxide) is to various oil and the adsorbance of organic reagent；
Figure 10 is large-scale production and the weave diagram thereof of continuous rope form material strip high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A that raw material poly(ethylene oxide) is prepared when being 1:1 with high density polyethylene (HDPE) mass ratio；
Figure 11 is the recycling experimental result picture of continuous rope form material strip high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A that raw material poly(ethylene oxide) is prepared when being 1:1 with high density polyethylene (HDPE) mass ratio.
Detailed description of the invention
By following example, the present invention is described in more details, but is not limiting as protection scope of the present invention.
In following example, high-density polyethylene number used is purchased from CNPC's Daqing petrochemical company for HDPE 5000S()；Poly(ethylene oxide) model used is that PEO POLYOX WSR N-10(is purchased from Dow Chemical company limited).
Embodiment
1
With poly(ethylene oxide) and the rheological experiment of the sample prepared by high density polyethylene (HDPE) of different quality ratio, comprise the following steps:
(1) poly(ethylene oxide) powder is mixed with deionized water, form it into pasty state (mass fraction of poly(ethylene oxide) is 40 ~ 50%), then pasty mixture is placed in baking oven, under the conditions of 30 ~ 40 DEG C be dried 2 ~ 3 days until its quality no longer changes, be broken for poly(ethylene oxide) pellet after being cooled to room temperature；
(2) the poly(ethylene oxide) pellet that step (1) is obtained with pellets of high density polyethylene with mass ratio as 1:9, the ratio of 1:4,1:2.3,1:1.5,1:1 is added separately in Minitype twin-screw extrusion machine melt extrude, the temperature melt extruded is 140 ~ 160 DEG C, and the rotating speed of screw rod is 8 ~ 12rpm；
(3) the continuous rope form material strip that step (2) melt extrudes is broken into pellet respectively, standby；
(4) pellet that step (3) obtains is utilized respectively vacuum film pressing machine, under conditions of temperature 150 DEG C, pressure 5MPa, is pressed into diameter 25mm, the disk of thickness 1mm, standby；
(5) disk step (4) obtained, under conditions of temperature 150 DEG C, strain 5%, utilizes rotational rheometer under the pattern of frequency scanning, tests its rheological property respectively, and result is as shown in Figure 1；
Fig. 1 is with poly(ethylene oxide) and high density polyethylene (HDPE) as raw material, preparing the rheometer test result of different samples during both mass ratio respectively 1:9,1:4,1:2.3,1:1.5,1:1, the storage modulus of the sample of the various proportionings obtained by rheometer test is with the situation of change of angular frequency.As can be seen from the figure, in low frequency range, increase along with dispersion phase poly(ethylene oxide) content, the value of storage modulus is consequently increased, beginning to decline after increasing to certain value, when the mass ratio of poly(ethylene oxide) Yu high density polyethylene (HDPE) is 1:1, the value of storage modulus is decreased obviously, this illustrates that the phase morphology of now sample interior there occurs change, island structure developed into co-continuous structure.I.e. can release from figure, what the mass ratio of raw material poly(ethylene oxide) and high density polyethylene (HDPE) was that the sample prepared when 1:9,1:4,1:2.3,1:1.5 presents is island structure, owing to there is not the cavernous structure of connection in the material of island structure, poor to the adsorption effect of oil；Raw material poly(ethylene oxide) is that the high density polyethylene (HDPE) oil-water separation material prepared during 1:1 the most most possibly forms co-continuous structure with the mass ratio of high density polyethylene (HDPE).
Embodiment
2
One of preparation method of high density polyethylene (HDPE) oil-water separation material, comprises the following steps:
(1) poly(ethylene oxide) powder is mixed with deionized water, form it into pasty state (mass fraction of poly(ethylene oxide) is 40 ~ 50%), then mixture is placed in baking oven, under the conditions of 35 ± 5 DEG C, dry 2 ~ 3 until its quality no longer changes, and is broken for poly(ethylene oxide) pellet after being cooled to room temperature；
(2) poly(ethylene oxide) pellet step (1) obtained joins in Minitype twin-screw extrusion machine with the pellets of high density polyethylene ratio with mass ratio as 1:1 and melt extrudes, and the temperature melt extruded is 140 ~ 160 DEG C, and the rotating speed of screw rod is 8 ~ 12rpm；
(3) continuous rope form material strip step (2) melt extruded, is collected under tensionless winkler foundation state with coiling machine, and the speed of collecting of coiling machine is 20 ± 2cm/min, the continuous material strip of the segment then continuous rope form material strip collected being cut into a length of 5 ~ 10cm；Sample is as shown in Figure 2 a；
(4) the continuous material strip of segment that step (3) obtains utilizes deionized water carry out supersound process at normal temperatures, and leaching removes water miscible poly(ethylene oxide), till the quality of segment material strip no longer changes；
(5) the continuous material strip of segment after step (4) leaching is placed in refrigerator freezing 2 ~ 5 hours under the conditions of-20 ~-15 DEG C；Freezing complete after in freezer dryer-85 ~-80 DEG C, vacuum be 0.4 ~ 1Pa under conditions of lyophilization 48 ~ 72 hours, obtain high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A；Sample A is as shown in Figure 2 b；
(6) Microstructure characterization: batten prepared by step (3) is quenched disconnected in liquid nitrogen, leaching removes water miscible poly(ethylene oxide) the most in deionized water, sample is put in refrigerator freezing by leaching after completing, subsequently the sample after freezing is placed in freezer dryer and is dried process, then by scanning electron microscope, the sample after being dried is detected, result is as shown in Figure 3, wherein 3a is high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A scanning electron microscope shape appearance figure along extrusion direction, Fig. 3 b is the partial enlarged drawing of Fig. 3 a；Fig. 3 c is the ultramicroscope shape appearance figure that high density polyethylene (HDPE) continuous tow is perpendicular to extrude direction, and Fig. 3 d is the partial enlarged drawing of Fig. 3 c.
Fig. 2 a Yu 2b is respectively high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A macroscopic form figure before and after being leached out poly(ethylene oxide): as can be seen from Figure, this sample there occurs large change before and after leaching, reason is that in this sample, poly(ethylene oxide) defines continuous phase before leaching, being conducive to deionized water to enter sample interior leaching from material strip top layer and remove more poly(ethylene oxide), therefore before and after leaching, tool changes significantly.
Fig. 3 a, 3b, 3c, 3d are the microscopic pattern figure of high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A, as seen from the figure: poly(ethylene oxide) and high density polyethylene (HDPE) mass ratio are high density polyethylene (HDPE) continuous tow prepared by 1:1, define three-dimensional porous structure, high density polyethylene (HDPE) presents the filamentary structure of orientations, the hole that Pluronic F-127 leaching is formed after removing communicates with each other, aperture is about between 1 μm to 20 μm, and such loose structure is conducive to the raising of oil absorbing effect.
Embodiment
3
The two of the preparation method of high density polyethylene (HDPE) continuous tow, comprise the following steps:
(1) poly(ethylene oxide) powder is mixed with deionized water, form it into pasty state (mass fraction of poly(ethylene oxide) is 40 ~ 50%), then mixture is placed in baking oven, under the conditions of 35 ± 5 DEG C be dried 2 ~ 3 days until its quality no longer changes, be broken for poly(ethylene oxide) pellet after being cooled to room temperature；
(2) poly(ethylene oxide) pellet step (1) obtained joins in Minitype twin-screw extrusion machine with the pellets of high density polyethylene ratio with mass ratio as 1:9 and melt extrudes, and the temperature melt extruded is 140 ~ 160 DEG C, and the rotating speed of screw rod is 8 ~ 12rpm；
(3) continuous rope form material strip step (2) melt extruded, is collected under tensionless winkler foundation state with coiling machine, and the speed of collecting of coiling machine is 20 ± 2cm/min, the continuous material strip of the segment then continuous rope form material strip collected being cut into a length of 5 ~ 10cm；Sample is as shown in fig. 4 a；
(4) the continuous material strip of segment that step (3) obtains utilizes deionized water carry out supersound process at normal temperatures, and leaching removes water miscible poly(ethylene oxide), till the quality of segment material strip no longer changes；
(5) the continuous material strip of segment after step (4) leaching is placed in refrigerator freezing 2 ~ 5 hours under the conditions of-20 ~-15 DEG C；Freezing complete after in freezer dryer-85 ~-80 DEG C, vacuum be 0.4 ~ 1Pa under conditions of lyophilization 48 ~ 72 hours, obtain high density polyethylene (HDPE) oil-water separation material B；Sample B is as shown in Figure 4 b；
(6) Microstructure characterization: batten prepared by step (3) is quenched disconnected in liquid nitrogen, leaching removes water miscible poly(ethylene oxide) the most in deionized water, sample is put in refrigerator freezing by leaching after completing, subsequently the sample after freezing is placed in freezer dryer and is dried process, then by scanning electron microscope, the sample after being dried is detected, result is as shown in Figure 5, wherein 5a is the high density polyethylene (HDPE) oil-water separation material B scanning electron microscope shape appearance figure along extrusion direction, and Fig. 5 b is the partial enlarged drawing of Fig. 5 a；Fig. 5 c is the ultramicroscope shape appearance figure that high density polyethylene (HDPE) oil-water separation material B is perpendicular to extrude direction, and Fig. 5 d is the partial enlarged drawing of Fig. 5 c.
As seen from the figure: poly(ethylene oxide) and high density polyethylene (HDPE) mass ratio are in the sample of high density polyethylene (HDPE) oil-water separation material B prepared by 1:9, before leaching, poly(ethylene oxide) is present in blend with the state of dispersion phase, present " island " shape structure one by one, do not communicate with each other between hole.
Embodiment
4
The five of the preparation method of a kind of high density polyethylene (HDPE) oil-water separation material, comprise the following steps:
(1) poly(ethylene oxide) powder is mixed with deionized water, form it into pasty state (mass fraction of poly(ethylene oxide) is 40 ~ 50%), then mixture is placed in baking oven, under the conditions of 35 ± 5 DEG C be dried 2 ~ 3 days until its quality no longer changes, be broken for poly(ethylene oxide) pellet after being cooled to room temperature；
(2) poly(ethylene oxide) pellet step (1) obtained joins in Minitype twin-screw extrusion machine with the pellets of high density polyethylene ratio with mass ratio as 1.5:1 and melt extrudes, and the temperature melt extruded is 140 ~ 160 DEG C, and the rotating speed of screw rod is 8 ~ 12rpm；
(3) continuous rope form material strip step (2) melt extruded, is collected under tensionless winkler foundation state with coiling machine, and the speed of collecting of coiling machine is 20 ± 2cm/min, the continuous material strip of the segment then continuous rope form material strip collected being cut into a length of 5 ~ 10cm；
(4) the continuous material strip of segment that step (3) obtains utilizes deionized water carry out supersound process at normal temperatures, and leaching removes water miscible poly(ethylene oxide), till the quality of segment material strip no longer changes；
(5) the continuous material strip of segment after step (4) leaching is placed in refrigerator freezing 2 ~ 5 hours under the conditions of-20 ~-15 DEG C；Freezing complete after in freezer dryer-85 ~-80 DEG C, vacuum be 0.4 ~ 1Pa under conditions of lyophilization 48 ~ 72 hours, obtain high density polyethylene (HDPE) oil-water separation material C；
Poly(ethylene oxide) is in the high density polyethylene (HDPE) oil-water separation material prepared during 1.5:1 with the mass ratio of high density polyethylene (HDPE), high density polyethylene (HDPE) is to be present in the matrix of poly(ethylene oxide) with the form of dispersion phase, owing to poly(ethylene oxide) is water miscible macromolecule, so after leaching experiment completes, poly(ethylene oxide) is leached, high density polyethylene (HDPE) is unable to maintain that complete structure because losing the supporting role of matrix, finally caves in, as shown in schematic diagram Fig. 6.
Embodiment
5
The application in oil-water separation of the high density polyethylene (HDPE) oil-water separation material of embodiment 2, embodiment 3 preparation.
High density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A embodiment 2 prepared respectively is suspended on iron stand with the high density polyethylene (HDPE) oil-water separation material B cotton thread of embodiment 3 preparation, sample is immersed in the vegetable oil with oil red dyeing, carries out oil suction experiment.As shown in Figure 7: the sample put on the right side of beaker in Fig. 7 is high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A prepared by embodiment 2, that put on the left of beaker is the high density polyethylene (HDPE) oil-water separation material B prepared by embodiment 3.
As can be seen from Figure: poly(ethylene oxide) is high density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A prepared by 1:1 with the mass ratio of high density polyethylene (HDPE), propelling over time, oil is gradually adsorbed up, until being full of whole sample, showing self-driven effect；Reason is that the high density polyethylene (HDPE) oil-water separation materials A poly(ethylene oxide) before leaching prepared communicates with each other mutually, so after being leached out poly(ethylene oxide), sample A is the formation of the loose structure of connection, the size of hole is in micron order, carry out oil suction experiment time will in capillarity under by oil absorption come up, i.e. show self-driven effect.And the mass ratio of poly(ethylene oxide) and high density polyethylene (HDPE) is high density polyethylene (HDPE) oil-water separation material B prepared by 1:9, oil absorption is not the most come up by carrying out over time；Reason be the high density polyethylene (HDPE) oil-water separation material B poly(ethylene oxide) before leaching prepared be to be present in the matrix of high density polyethylene (HDPE) with dispersion phase, poly(ethylene oxide) does not the most connect, when carrying out leaching, deionized water is difficult to enter into sample interior, also the loose structure of connection cannot be formed, so oil absorption can not be come up by this result.
In Fig. 8: with the hexamethylene dyeed with oil red on the high density polyethylene (HDPE) oil-water separation materials A absorption water surface.As can be seen from the figure the hexamethylene on the water surface can be adsorbed by high density polyethylene (HDPE) oil-water separation materials A completely, illustrates that this sample has good oil-water separation characteristic.
High density polyethylene (HDPE) oil-water separation material (high density polyethylene (HDPE) continuous tow) A that poly(ethylene oxide) is prepared when being 1:1 from the mass ratio of high density polyethylene (HDPE) has different absorbabilitys to various oil, organic reagent, to the absorbability of different material as shown in Figure 9.By result in Fig. 9 it can be seen that high density polyethylene (HDPE) oil-water separation materials A can adsorb the soybean oil being equivalent to own wt 438%, the machine oil of 450%, the silicone oil of 425%, the hexamethylene of 300%, the chloroform of 431%, i.e. this sample have preferable absorbability for various oil and organic reagent.
From above content: with poly(ethylene oxide) and high density polyethylene (HDPE) as raw material, use simple to operate, environmentally safe melt extrudes method when preparing high density polyethylene (HDPE) oil-water separation material, the mass ratio of poly(ethylene oxide) and high density polyethylene (HDPE) be the high density polyethylene (HDPE) oil-water separation material prepared during 1:1 be high-density polyethylene continuous alkene fibre bundle, present continuous print loose structure, multiple oil and organic reagent are had preferable adsorption.The product using the method to prepare has rope form three-dimensional porous structure; soft continuously, can weave; as shown in Figure 10; the method not only achieves continuous large-scale production; simple preparation method can be used to realize the large-scale production and application of this product, and its fabric as administering Crude Oil at Sea leakage and can purify the ideal material of oil-containing sanitary sewage.
Embodiment
6
The performance detection of the high density polyethylene (HDPE) oil-water separation materials A hdpe fiber bundle sample prepared for 1:1 with high density polyethylene (HDPE) mass ratio with poly(ethylene oxide), has following steps:
(1) use the hdpe fiber bundle absorption soybean oil of preparation, be centrifuged processing, sloughing the waste oil of absorption in sample to the sample after oil suction with centrifuge again after completing absorption, waste oil is collected；
(2) the hdpe fiber Shu Zaici after step (1) centrifugal treating is used to adsorb soybean oil, i.e. recycling hdpe fiber bundle；Again it is centrifuged after completing absorption processing, recycles successively；
(3) testing the high density polyethylene (HDPE) continuous tow after oil suction in step (1) and step (2) and the high density polyethylene (HDPE) continuous tow after centrifugal treating, result is as shown in figure 11.
In fig. 11, in figure, square symbol horizontal line represents the high density polyethylene (HDPE) continuous tow adsorbance to soybean oil；Circle symbol horizontal line represents high density polyethylene (HDPE) continuous tow after oil suction carrying out centrifugal treating, the residual quantity of soybean oil in sample.As can be seen from the figure, within circulating at 100, although high density polyethylene (HDPE) continuous tow is for some fluctuation of adsorbance of soybean oil, but substantially maintain in the range of 400 ~ 500%, and in when using for the 100th time, this sample remains within the adsorption range of 400 ~ 500% to the adsorbance of oil, do not significantly decrease, advantages of good adsorption effect；After centrifugal treating, in high density polyethylene (HDPE) continuous tow, the residual quantity of soybean oil is then maintained at relatively low level, the soybean oil having more than 90% is divested by centrifugal process, residual quantity when the 100th time is the most little, the high density polyethylene (HDPE) continuous tow i.e. using the inventive method to prepare has good repetitive cycling utilizing status, also achieves the recycling of waste oil simultaneously.
Claims (10)
1. the preparation method of a high density polyethylene (HDPE) oil-water separation material, it is characterised in that comprise the following steps:
(1) poly(ethylene oxide) powder and deionized water are mixed to form pasty state, then mixture are placed in baking oven and dry until its quality no longer changes, after being cooled to room temperature, be broken for poly(ethylene oxide) pellet；
(2) join extruder melt extrudes by the poly(ethylene oxide) pellet obtained in step (1) and pellets of high density polyethylene and obtain continuous rope form material strip；Wherein the mass fraction shared by poly(ethylene oxide) is 10 ~ 60%；
(3) continuous rope form material strip step (2) melt extruded, is collected under tensionless winkler foundation state with coiling machine, and the continuous rope form material strip collected is cut into the continuous material strip of segment；
(4) segment continuous rope form material strip step (3) obtained utilizes deionized water to carry out supersound process at normal temperatures, and leaching removes water miscible poly(ethylene oxide), till the quality of the continuous material strip of segment no longer changes；
(5) the continuous material strip of segment after the leaching that will obtain in step (4) is placed in refrigerator freezing, and freezing is dried process after completing in freezer dryer, obtains high density polyethylene (HDPE) oil-water separation material, detects.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that the molecular weight of described poly(ethylene oxide) powder is 100000 ~ 200000.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that when step (1) described poly(ethylene oxide) powder mixes with deionized water, the mass fraction of poly(ethylene oxide) is 40 ~ 50%.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that the baking temperature of the oven drying described in step (1) is 30 ~ 40 DEG C, drying time is 2 ~ 3 days；The particle diameter of the described broken poly(ethylene oxide) pellet obtained is 0.8 ~ 1.2mm.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that the mass fraction shared by step (2) described poly(ethylene oxide) is 50%.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 5, it is characterized in that, described high density polyethylene (HDPE) oil-water separation material is high density polyethylene (HDPE) continuous tow, and described high density polyethylene (HDPE) continuous tow has a diameter of 1 μm hole to 20 μm.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that the extruder described in step (2) is Minitype twin-screw extrusion machine；When described raw material melt extrudes in an extruder, the temperature melt extruded is 140 ~ 160 DEG C, the rotating speed of extruder screw is 8 ~ 12rpm；Step (3) described coiling machine is when being collected, and the speed of collecting of coiling machine is 20 ± 2cm/min.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that step (5) described material strip cryogenic temperature in refrigerator is-20 ~-15 DEG C, cooling time is 2 ~ 5 hours；Temperature when being dried in freezer dryer is-85 ~-80 DEG C, vacuum is 0.4 ~ 1Pa, and the cryodesiccated time is 48 ~ 72 hours.
The preparation method of high density polyethylene (HDPE) oil-water separation material the most according to claim 1, it is characterised in that described high density polyethylene (HDPE) oil-water separation material application in oil-water separation.
10. a high density polyethylene (HDPE) oil-water separation material, it is characterised in that described high density polyethylene (HDPE) oil-water separation material is to be prepared by the method according to any one of claim 1 ~ 9.
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| CN108715647A (en) * | 2018-05-24 | 2018-10-30 | 四川大学 | Polyethylene biofilm carrier material and preparation method thereof |
| CN112337137A (en) * | 2020-10-19 | 2021-02-09 | 中国人民警察大学 | Preparation method and application of novel magnetic spilled oil pollution decontamination material |
| CN113491956A (en) * | 2021-07-15 | 2021-10-12 | 河南工程学院 | LLDPE oil-water separation membrane and preparation method and application thereof |
| CN115722209A (en) * | 2022-09-27 | 2023-03-03 | 东华大学 | Polyoxymethylene microfiber oil-water separation material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108715647A (en) * | 2018-05-24 | 2018-10-30 | 四川大学 | Polyethylene biofilm carrier material and preparation method thereof |
| CN108715647B (en) * | 2018-05-24 | 2021-08-06 | 四川大学 | Polyethylene biological film carrier material and preparation method thereof |
| CN112337137A (en) * | 2020-10-19 | 2021-02-09 | 中国人民警察大学 | Preparation method and application of novel magnetic spilled oil pollution decontamination material |
| CN113491956A (en) * | 2021-07-15 | 2021-10-12 | 河南工程学院 | LLDPE oil-water separation membrane and preparation method and application thereof |
| CN115722209A (en) * | 2022-09-27 | 2023-03-03 | 东华大学 | Polyoxymethylene microfiber oil-water separation material and preparation method thereof |
| CN115722209B (en) * | 2022-09-27 | 2024-04-12 | 东华大学 | Polyoxymethylene microfiber oil-water separation material and preparation method thereof |
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