CN105906909B - A kind of high density polyethylene (HDPE) water-oil separating material and preparation method thereof - Google Patents
A kind of high density polyethylene (HDPE) water-oil separating material and preparation method thereof Download PDFInfo
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- CN105906909B CN105906909B CN201610330833.3A CN201610330833A CN105906909B CN 105906909 B CN105906909 B CN 105906909B CN 201610330833 A CN201610330833 A CN 201610330833A CN 105906909 B CN105906909 B CN 105906909B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses a kind of high density polyethylene (HDPE) water-oil separating materials and preparation method thereof.The present invention is using polyethylene oxide and high density polyethylene (HDPE) as raw material, by extruder melting extrusion, carried out batching collection by coiling machine, then leaching is carried out with sample of the deionized water to collection remove polyethylene oxide, freeze-drying process is carried out by refrigerator and freeze drier again, obtain high density polyethylene (HDPE) water-oil separating material, this method simple process, time is short, without using chemicals no pollution to the environment, at low cost.It include the structure of high density polyethylene (HDPE) continuous tow using high density polyethylene (HDPE) water-oil separating material prepared by this method, the structure has the hole that diameter is several microns to more than ten microns, shows porous orientation fibrous structure, has preferable suction-operated to oil and organic reagent；The sample length is continuous, water-oil separating fabric that is soft, being woven into large area, provides effective solution method to administer Crude Oil at Sea leakage and purifying domestic sewage.
Description
Technical field
The invention belongs to new materials to process preparation field, be related to a kind of preparation method of three-dimensional porous water-oil separating material
More particularly to a kind of high density polyethylene (HDPE) water-oil separating material and preparation method thereof.
Background technique
Come in administer Crude Oil at Sea leakage and purification oil-containing sanitary sewage is faced with increasing challenge, current improvement
Method is probably divided into following several：Using on the material recovery water surface of hydrophobic oleophilic oil property oil, using dispersing agent grease is mixed
It closes to promote its natural degradation, directly burning to remove oil slick.The method that ordinary priority considers is using with hydrophobic oleophilic oil
The material of matter recycles slick, because can deal carefully with oil slick in this way, will not occur secondary pollution again.Make at present
The material of these hydrophobic oleophilic oils 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, due to can provide storage with gap structure abundant
The space of oil product keeps the oil absorption capacity of material larger, has significant advantage in practical applications.2004 Nian Jiang thunder seminars are first
It is secondary that super-hydrophobic concept is introduced into the application of water-oil separating, and it is successfully prepared the metal grill of super-hydrophobic super-oleophylic；Grandson
Li Tao seminar heat-treated under the conditions of the aqueous dispersions of graphite oxide are placed in 180 DEG C using the method for chemical reaction 24 hours it
Graphene hydrogel is formed afterwards, hydrogel is then obtained into graphene aerogel by freeze-drying, the aeroge being prepared
With porous structure and hydrophobic -- the mechanical strength of oil-wet behavior, this three-dimensional porous hydrophobic material is poor, and three-dimensional framework cannot
Deformation occurs or is easier to pulverized destruction, and applicability is lower in the complex environment for actually carrying out water-oil separation；Tsinghua University
The sea Wu De seminar passes through the fast package material of carbon nanotube that chemical vapour deposition technique is prepared for three-dimensional porous sponge shape, carbon nanotube
Sponge has superhydrophobic characteristic, and gap structure abundant and ultralight density make material have stronger oil absorption capacity, can absorb
The amount of organic solvent or oil product is about 80 ~ 180 times of own wt, but preparation method is complicated, at high cost；And the prior art
Common electrospinning process needs the addition of organic solvent, harmful to human strong when preparing water-oil separating material using this method
Health, environmental pollution, and preparation time is long, reduces production efficiency and is unfavorable for large-scale industrial production application.The above method is equal
Three-dimensional porous water-oil separating material is prepared, but these preparation methods have preparation process complexity, use chemical reagent
It causes environmental pollution, be difficult to the characteristics of large-scale production and application, be unfavorable for instructing industrialized production.
High density polyethylene (HDPE)（HDPE）It is one of most widely used general-purpose plastics, it is cheap and easy to get, performance is stable, preparation
Technology maturation, and high density polyethylene (HDPE) belongs to environmental-protecting material, heating reaches fusing point can recycling and reusing.High density polyethylene (HDPE) sheet
Body has the property of hydrophobic oleophilic oil, is processed into after three-dimensional porous material, water-oil separating can be more effectively carried out, with it
His water-oil separation material（Such as carbon nanotube sponge, graphene aerogel）It compares, it is easily processed into type, preparation cost is low,
It can be used repeatedly, be conducive to large-scale continuous production, be suitable for industrial applications.But high density polyethylene (HDPE) is processed at present
More complicated preparation method and equipment, higher cost is needed to be unfavorable for large-scale production and application for water-oil separating material.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation method of high density polyethylene (HDPE) water-oil separating material,
This method process flow is simple, easy to operate, and without the addition, environmental-friendly of chemicals, production cost is low, can connect on a large scale
Continuous production application.
It the use of water-oil separating material prepared by the method for the present invention include high density polyethylene (HDPE) continuous tow structure, the fiber
Beam shows porous orientation fibrous structure, can be compiled into the water-oil separating fabric of large area, has efficient water-oil separating
Effect.
The present invention is achieved by the following technical solutions
A kind of preparation method of high density polyethylene (HDPE) water-oil separating material, includes the following steps：
（1）Polyethylene oxide powder and deionized water are mixed to form paste, then mixture is placed in baking oven and is dried
Until its quality is no longer changed, polyethylene oxide pellet is broken for after being cooled to room temperature；
（2）By step（1）Obtained polyethylene oxide pellet is added in extruder with pellets of high density polyethylene to be melted
Extrusion obtains continuous rope form material strip；Wherein mass fraction shared by polyethylene oxide is 10 ~ 60%；
（3）By step（2）The continuous rope form material strip of melting extrusion is collected under tensionless winkler foundation state with coiling machine, and
The continuous rope form material strip being collected into is cut into the continuous material strip of segment；
（4）By step（3）The continuous rope form material of obtained segment is ultrasonically treated using deionized water at normal temperature, leaching
Water-soluble polyethylene oxide is removed, until the quality of the continuous material strip of segment is no longer changed；
（5）By step（4）Obtained in the continuous material strip of segment after leaching be placed in refrigerator and freeze, after the completion of freezing
It is dried to obtain high density polyethylene (HDPE) water-oil separating material in freeze drier, be detected.
The molecular weight of the preparation method of the high density polyethylene (HDPE) water-oil separating material, the polyethylene oxide powder is
100000 ~ 200000, it is polyethylene glycol oxide PEO.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, step（1）The polyethylene oxide powder
When mixing with deionized water, the mass fraction of polyethylene oxide is 40 ~ 50%.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, step（1）The drying of the oven drying
Temperature is 30 ~ 40 DEG C, drying time is 2 ~ 3 days；The partial size of the broken obtained polyethylene oxide pellet is 0.8 ~ 1.2mm.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, step（2）Shared by the polyethylene oxide
Mass fraction is 50%.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, the high density polyethylene (HDPE) water-oil separating material
Material is high density polyethylene (HDPE) continuous tow, and it is 1 μm to 20 μm that the high density polyethylene (HDPE) continuous tow, which has diameter,
Hole.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, step（2）The extruder is miniature double
Screw extruder；The raw material in an extruder melting extrusion when, the temperature of melting extrusion is 140 ~ 160 DEG C, extruder screw
Revolving speed be 8 ~ 12rpm；Step（3）For the coiling machine when being collected, the rate of collecting of coiling machine is 20 ± 2cm/min.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, step（5）The material strip freezes in refrigerator
Temperature be -20 ~ -15 DEG C, cooling time be 2 ~ 5 hours；Temperature when dry in refrigerator is -85 ~ -80 DEG C, vacuum
Degree is 0 ~ 1pa, and the time of freeze-drying is 48 ~ 72 hours.
The preparation method of the high density polyethylene (HDPE) water-oil separating material, the high density polyethylene (HDPE) water-oil separating material
Expect the application in water-oil separating.
A kind of high density polyethylene (HDPE) water-oil separating material, the high density polyethylene (HDPE) water-oil separating material is by above-mentioned
Method preparation.
The present invention by polyethylene oxide and high density polyethylene (HDPE) with different mass ratio mixing extrusion moldings, then by go from
Sub- water leaching removes polyethylene oxide, forms the water-oil separating material of different structure.When polyethylene oxide and high density polyethylene (HDPE)
Mass ratio be 1:When 1, the hdpe fiber beam being made of fento is formed.Utilize method for processing forming-extrusion molding
And the method for leaching carrys out processing and forming high density polyethylene (HDPE) water-oil separating material, has process operation easy, at low cost, uses
Raw material without containing chemicals, no pollution to the environment, at low cost, product is soft, length is continuous, can be mass-produced using etc. it is excellent
Point.The material being prepared has preferable oil-water separation.
Compared with prior art, the present invention has following positive beneficial effect：
（1）The present invention is prepared for high density polyethylene (HDPE) water-oil separating material using the method for extrusion molding and leaching, solution
The problem of serialization, scale, the low cost porous water-oil separating material of production are difficult in existing preparation method of having determined；
（2）It is prepared using preparation method of the invention raw materials used honest and clean during high density polyethylene (HDPE) water-oil separating material
Valence is easy to get, the addition of not no chemicals, pollution-free and greatly reduce production cost, process safety and environmental protection；
（3）Preparation method through the invention can prepare the high-density polyethylene being made of fento for water-oil separating
Alkene continuous tow, the size of hole are micro-meter scale, which shows porous orientation fibrous structure, with higher
Adsorption efficiency；The polyethylene continuous tow length is continuous, soft, can be woven into the water-oil separating fabric of large area, to administer
Crude Oil at Sea leakage and purification oil-containing sanitary sewage provide effective solution method；
（4）The present invention is used in water-oil separating application using the hdpe fiber beam of extruding forming method preparation
Service life is long, after passing through centrifugal treating after the material oil suction, can be reused for water-oil separating, still have well
Oil absorbing effect, repetitive cycling can still be maintained good oil absorbing effect using 100 times, not only greatly reduce water-oil separating
Cost, the collection for also achieving waste oil recycle, economic results in society with higher.
Detailed description of the invention
Fig. 1 is the energy storage for the different samples that raw material polyethylene oxide and high density polyethylene (HDPE) are prepared when different quality matches
Modulus with angular frequency situation of change；
Fig. 2 is that the mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) grease prepared when 1 point
From material（High density polyethylene (HDPE) continuous tow）The macroscopic form figure of A, it is macro before wherein Fig. 2 a is leaching polyethylene oxide
Figure is seen, 2b is the macroscopic form figure after leaching polyethylene oxide；
Fig. 3 is that the mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) grease prepared when 1 point
From material（High density polyethylene (HDPE) continuous tow）The micromorphology figure of A, wherein Fig. 3 a is high density polyethylene (HDPE) continuous tow
For sample A along the scanning electron microscope shape appearance figure for squeezing out direction, Fig. 3 b is the partial enlarged view of Fig. 3 a；Fig. 3 c is poly- for high density
For ethylene continuous tow A perpendicular to the electron microscope shape appearance figure for squeezing out direction, Fig. 3 d is the partial enlarged view of Fig. 3 c；
Fig. 4 is the mass ratio 1 of polyethylene oxide and high density polyethylene (HDPE):The high density polyethylene (HDPE) water-oil separating prepared when 9
The macroscopic form figure of material B, the macrograph before wherein Fig. 4 a is leaching ethylene oxide, Fig. 4 b is after leaching ethylene oxide
Macroscopic form figure；
The mass ratio of Fig. 5 polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) water-oil separating prepared when 9
The micromorphology figure of material B, wherein Fig. 5 a is high density polyethylene (HDPE) water-oil separating material B aobvious along the scanning electron for squeezing out direction
Micro mirror shape appearance figure, Fig. 5 b are the enlarged drawing of Fig. 5 a；Fig. 5 c is high density polyethylene (HDPE) water-oil separating material B perpendicular to extrusion direction
Scanning electron microscope shape appearance figure, Fig. 5 d are the enlarged drawing of Fig. 5 c；
Fig. 6 is respectively 1 for the mass ratio of raw material polyethylene oxide and high density polyethylene (HDPE):9,1:1,1.5:It is prepared when 1
Structural schematic diagram of the product high density polyethylene (HDPE) water-oil separating material before and after leaching；
Fig. 7 is that the mass ratio of raw material polyethylene oxide and high density polyethylene (HDPE) is 9:1（Continuous material strip on the left of beaker）And
Mass ratio is 1:1（Continuous material strip on the right side of beaker）When the oil suction dynamic contrast of high density polyethylene (HDPE) water-oil separating material for preparing
Figure；
Fig. 8 is that the mass ratio of raw material polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) oil prepared when 1
Water separation material（High density polyethylene (HDPE) continuous tow）The lab diagram of A progress water-oil separating；
Fig. 9 is raw material polyethylene oxide and high density polyethylene (HDPE) mass ratio is 1:The continuous rope form material strip prepared when 1 is highly dense
Spend polyethylene water-oil separating material（High density polyethylene (HDPE) continuous tow）Adsorbance of the A to various oil and organic reagent；
Figure 10 is raw material polyethylene oxide and high density polyethylene (HDPE) mass ratio is 1:The continuous rope form material strip prepared when 1 is highly dense
Spend polyethylene water-oil separating material（High density polyethylene (HDPE) continuous tow）The large-scale production and its weave diagram of A；
Figure 11 is raw material polyethylene oxide and high density polyethylene (HDPE) mass ratio is 1:The continuous rope form material strip prepared when 1 is highly dense
Spend polyethylene water-oil separating material（High density polyethylene (HDPE) continuous tow）The recycling experimental result picture of A.
Specific embodiment
The present invention is described in more details by following embodiment, but is not intended to limit protection model of the invention
It encloses.
In following embodiment, high-density polyethylene number used is HDPE 5000S（Purchased from China Petroleum grand celebration stone
Change company）；Polyethylene oxide model PEO POLYOX WSR N-10 used（Purchased from Dow Chemical Co., Ltd）.
Embodiment 1
With the rheological experiment of sample prepared by the polyethylene oxide of different quality ratio and high density polyethylene (HDPE), including it is following
Step：
（1）Polyethylene oxide powder is mixed with deionized water, forms it into paste（The mass fraction of polyethylene oxide is
40~50%）, then pasty mixture is placed in baking oven, is dried 2 ~ 3 days under the conditions of 30 ~ 40 DEG C until its quality no longer occurs
Variation, is broken for polyethylene oxide pellet after being cooled to room temperature；
（2）By step（1）Obtained polyethylene oxide pellet and pellets of high density polyethylene is with mass ratio for 1:9,1:4,
1:2.3,1:1.5,1:1 ratio is added separately to melting extrusion in Minitype twin-screw extrusion machine, and the temperature of melting extrusion is
140 ~ 160 DEG C, the revolving speed of screw rod is 8 ~ 12rpm；
（3）By step（2）The continuous rope form material strip of melting extrusion is broken into pellet respectively, spare；
（4）By step（3）Obtained pellet is utilized respectively vacuum film pressing machine, in 150 DEG C of temperature, the condition of pressure 5MPa
Under, it is pressed into the disk of diameter 25mm, thickness 1mm, it is spare；
（5）By step（4）Obtained disk, at 150 DEG C of temperature, under conditions of strain 5%, using rotational rheometer in frequency
Under the mode of rate scanning, its rheological property is tested respectively, as a result as shown in Figure 1；
Fig. 1 is using polyethylene oxide and high density polyethylene (HDPE) as raw material, and the two mass ratio is respectively 1:9,1:4,1:2.3,
1:1.5,1：The rheometer test of different samples is prepared when 1 as a result, the sample of the various proportions obtained by rheometer test storage
Can modulus with angular frequency situation of change.It can be seen from the figure that in low frequency range, with the increasing of dispersed phase polyethylene oxide content
Add, the value of storage modulus is consequently increased, and is begun to decline after increasing to certain value, when polyethylene oxide and high density polyethylene (HDPE)
Mass ratio be 1：When 1, the value of storage modulus is decreased obviously, this illustrates that the phase morphology of sample interior at this time is changed, by
Island structure has evolved into co-continuous structure.It can be released i.e. from figure, the matter of raw material polyethylene oxide and high density polyethylene (HDPE)
Amount is than being 1:9,1:4,1:2.3,1:What the sample prepared when 1.5 was presented is island structure, and the material of island structure is not due to depositing
It is poor to the adsorption effect of oil in the cavernous structure of connection；The mass ratio of raw material polyethylene oxide and high density polyethylene (HDPE) is
1:The high density polyethylene (HDPE) water-oil separating material prepared when 1 then most possibly forms co-continuous structure.
Embodiment 2
One of the preparation method of high density polyethylene (HDPE) water-oil separating material, includes the following steps：
（1）Polyethylene oxide powder is mixed with deionized water, forms it into paste（The mass fraction of polyethylene oxide is
40~50%）, then mixture is placed in baking oven, dry 2 ~ 3 until its quality is no longer changed under the conditions of 35 ± 5 DEG C,
Polyethylene oxide pellet is broken for after being cooled to room temperature；
（2）By step（1）Obtained polyethylene oxide pellet and pellets of high density polyethylene is with mass ratio for 1:1 ratio
It is added to melting extrusion in Minitype twin-screw extrusion machine, the temperature of melting extrusion is 140 ~ 160 DEG C, the revolving speed of screw rod is 8 ~
12rpm；
（3）By step（2）The continuous rope form material strip of melting extrusion is collected under tensionless winkler foundation state with coiling machine, volume
The rate of collecting for taking machine is 20 ± 2cm/min, and it is the small of 5 ~ 10cm that the continuous rope form material strip being collected into, which is then cut into length,
Duan Lianxu material strip；Sample is as shown in Figure 2 a；
（4）By step（3）The continuous material strip of obtained segment is ultrasonically treated using deionized water at normal temperature, and leaching removes
Water-soluble polyethylene oxide is gone, until the quality of segment material strip is no longer changed；
（5）By step（4）The continuous material strip of segment after leaching is placed in refrigerator freezes 2 ~ 5 under the conditions of -20 ~ -15 DEG C
Hour；After the completion of freezing in freeze drier -85 ~ -80 DEG C, vacuum degree be 0.4 ~ 1Pa under conditions of freeze-drying 48 ~
72 hours, obtain high density polyethylene (HDPE) water-oil separating material（High density polyethylene (HDPE) continuous tow）A；Sample A is as shown in Figure 2 b；
（6）Microstructure characterization：By step（3）The batten of preparation is quenched disconnected, then leaching in deionized water in liquid nitrogen
Water-soluble polyethylene oxide is removed, sample is put into refrigerator after the completion of leaching and is freezed, is then placed in the sample after freezing
It is dried, then the sample after drying is detected with scanning electron microscope, as a result such as in freeze drier
Shown in Fig. 3, wherein 3a is high density polyethylene (HDPE) water-oil separating material（High density polyethylene (HDPE) continuous tow）A is along extrusion direction
Scanning electron microscope shape appearance figure, Fig. 3 b be Fig. 3 a partial enlarged view；Fig. 3 c hangs down for high density polyethylene (HDPE) continuous tow
Directly in the electron microscope shape appearance figure for squeezing out direction, Fig. 3 d is the partial enlarged view of Fig. 3 c.
Fig. 2 a and 2b is respectively high density polyethylene (HDPE) water-oil separating material（High density polyethylene (HDPE) continuous tow）A is being dripped
Filter the macroscopic form figure before and after polyethylene oxide：As can be seen from Figure, which is varied widely before and after leaching,
The reason is that polyethylene oxide forms continuous phase in the sample before leaching, is conducive to deionized water from material strip surface layer and enters sample
Internal leaching removes more polyethylene oxide, therefore tool changes significantly before and after leaching.
Fig. 3 a, 3b, 3c, 3d are high density polyethylene (HDPE) water-oil separating material（High density polyethylene (HDPE) continuous tow）A's is micro-
Aspect graph is seen, as seen from the figure：Polyethylene oxide and high density polyethylene (HDPE) mass ratio are 1:The high density polyethylene (HDPE) of 1 preparation connects
Continuous fibre bundle, forms three-dimensional porous structure, high density polyethylene (HDPE) shows the fibrous structure of orientations, Pluronic F-127
The hole that leaching is formed after removing communicates with each other, and about between 1 μm to 20 μm, such porous structure is conducive in aperture
The raising of oil absorbing effect.
Embodiment 3
The two of the preparation method of high density polyethylene (HDPE) continuous tow, include the following steps：
（1）Polyethylene oxide powder is mixed with deionized water, forms it into paste（The mass fraction of polyethylene oxide is
40~50%）, then mixture is placed in baking oven, is dried 2 ~ 3 days under the conditions of 35 ± 5 DEG C until its quality no longer becomes
Change, polyethylene oxide pellet is broken for after being cooled to room temperature；
（2）By step（1）Obtained polyethylene oxide pellet and pellets of high density polyethylene is with mass ratio for 1:9 ratio
It is added to melting extrusion in Minitype twin-screw extrusion machine, the temperature of melting extrusion is 140 ~ 160 DEG C, the revolving speed of screw rod is 8 ~
12rpm；
（3）By step（2）The continuous rope form material strip of melting extrusion is collected under tensionless winkler foundation state with coiling machine, volume
The rate of collecting for taking machine is 20 ± 2cm/min, and it is the small of 5 ~ 10cm that the continuous rope form material strip being collected into, which is then cut into length,
Duan Lianxu material strip；Sample is as shown in fig. 4 a；
（4）By step（3）The continuous material strip of obtained segment is ultrasonically treated using deionized water at normal temperature, and leaching removes
Water-soluble polyethylene oxide is gone, until the quality of segment material strip is no longer changed；
（5）By step（4）The continuous material strip of segment after leaching is placed in refrigerator freezes 2 ~ 5 under the conditions of -20 ~ -15 DEG C
Hour；After the completion of freezing in freeze drier -85 ~ -80 DEG C, vacuum degree be 0.4 ~ 1Pa under conditions of freeze-drying 48 ~
72 hours, obtain high density polyethylene (HDPE) water-oil separating material B；Sample B is as shown in Figure 4 b；
（6）Microstructure characterization：By step（3）The batten of preparation is quenched disconnected, then leaching in deionized water in liquid nitrogen
Water-soluble polyethylene oxide is removed, sample is put into refrigerator after the completion of leaching and is freezed, is then placed in the sample after freezing
It is dried, then the sample after drying is detected with scanning electron microscope, as a result such as in freeze drier
Shown in Fig. 5, wherein 5a is scanning electron microscope shape appearance figure of the high density polyethylene (HDPE) water-oil separating material B along extrusion direction,
Fig. 5 b is the partial enlarged view of Fig. 5 a；Fig. 5 c is high density polyethylene (HDPE) water-oil separating material B perpendicular to the electronic display for squeezing out direction
Micro mirror shape appearance figure, Fig. 5 d are the partial enlarged view of Fig. 5 c.
As seen from the figure：Polyethylene oxide and high density polyethylene (HDPE) mass ratio are 1:The high density polyethylene (HDPE) oil of 9 preparations
In the sample of water separation material B, polyethylene oxide is present in blend before leaching with the state of dispersed phase, shows one one
A " island " shape structure does not communicate with each other between hole.
Embodiment 4
The five of a kind of preparation method of high density polyethylene (HDPE) water-oil separating material, include the following steps：
（1）Polyethylene oxide powder is mixed with deionized water, forms it into paste（The mass fraction of polyethylene oxide is
40~50%）, then mixture is placed in baking oven, is dried 2 ~ 3 days under the conditions of 35 ± 5 DEG C until its quality no longer becomes
Change, polyethylene oxide pellet is broken for after being cooled to room temperature；
（2）By step（1）Obtained polyethylene oxide pellet and pellets of high density polyethylene is with mass ratio for 1.5:1 ratio
Example is added to melting extrusion in Minitype twin-screw extrusion machine, and the temperature of melting extrusion is 140 ~ 160 DEG C, and the revolving speed of screw rod is 8 ~
12rpm；
（3）By step（2）The continuous rope form material strip of melting extrusion is collected under tensionless winkler foundation state with coiling machine, volume
The rate of collecting for taking machine is 20 ± 2cm/min, and it is the small of 5 ~ 10cm that the continuous rope form material strip being collected into, which is then cut into length,
Duan Lianxu material strip；
（4）By step（3）The continuous material strip of obtained segment is ultrasonically treated using deionized water at normal temperature, and leaching removes
Water-soluble polyethylene oxide is gone, until the quality of segment material strip is no longer changed；
（5）By step（4）The continuous material strip of segment after leaching is placed in refrigerator freezes 2 ~ 5 under the conditions of -20 ~ -15 DEG C
Hour；After the completion of freezing in freeze drier -85 ~ -80 DEG C, vacuum degree be 0.4 ~ 1Pa under conditions of freeze-drying 48 ~
72 hours, obtain high density polyethylene (HDPE) water-oil separating material C；
The mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1.5:The high density polyethylene (HDPE) water-oil separating material prepared when 1
In material, high density polyethylene (HDPE) is present in the matrix of polyethylene oxide in the form of dispersed phase, since polyethylene oxide is water
The macromolecule of dissolubility, so polyethylene oxide is leached, and high density polyethylene (HDPE) is because losing matrix after leaching experiment completion
Supporting role and be unable to maintain that complete structure, it is final to collapse, as shown in schematic diagram Fig. 6.
Embodiment 5
The application of high density polyethylene (HDPE) water-oil separating material prepared by embodiment 2, embodiment 3 in water-oil separating.
The high density polyethylene (HDPE) water-oil separating material respectively prepared by embodiment 2（High density polyethylene (HDPE) continuous tow）A
The high density polyethylene (HDPE) water-oil separating material B prepared with embodiment 3 is suspended on iron stand with cotton thread, and sample is immersed in oil
In the vegetable oil of red colouring, oil suction experiment is carried out.As shown in Figure 7：The sample being put on the right side of beaker in Fig. 7 is to be made by embodiment 2
Standby high density polyethylene (HDPE) water-oil separating material（High density polyethylene (HDPE) continuous tow）A, what beaker left side was put into is by implementing
High density polyethylene (HDPE) water-oil separating material B prepared by example 3.
As can be seen from Figure：The mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1:The high-density polyethylene of 1 preparation
Alkene water-oil separating material（High density polyethylene (HDPE) continuous tow）A, with the propulsion of time, oil is gradually adsorbed up until filling
Full entire sample is shown from driving effect；The reason is that the high density polyethylene (HDPE) water-oil separating material A of preparation gathers before leaching
Ethylene oxide mutually communicates with each other, so sample A is formed the porous knot of connection after being leached out polyethylene oxide
The size of structure, hole is in micron order, oil absorption will come up under capillarity when carrying out oil suction experiment, that is, show
Come from driving effect.And the mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) grease point of 9 preparations
From material B, as the progress of time does not always come up oil absorption；The reason is that the high density polyethylene (HDPE) water-oil separating material of preparation
Expect B polyethylene oxide before leaching be to be present in the matrix of high density polyethylene (HDPE) with dispersed phase, polyethylene oxide each other it
Between be not connected to, carry out leaching when deionized water be difficult to enter sample interior, cannot also form the porous structure of connection, institute
Oil absorption cannot be come up with the result.
In Fig. 8：With the hexamethylene dyed on the high density polyethylene (HDPE) water-oil separating material A absorption water surface with oil red.From figure
It can be seen that high density polyethylene (HDPE) water-oil separating material A can adsorb completely the hexamethylene on the water surface, illustrate that the sample has
Good water-oil separating characteristic.
The mass ratio of polyethylene oxide and high density polyethylene (HDPE) is 1:The high density polyethylene (HDPE) water-oil separating material prepared when 1
（High density polyethylene (HDPE) continuous tow）A has different adsorption capacities to various oil, organic reagent, the absorption to different material
Ability is as shown in Figure 9.It can be seen that by result in Fig. 9：High density polyethylene (HDPE) water-oil separating material A, which can be adsorbed, is equivalent to itself
The soybean oil of weight 438%, 450% machine oil, 425% silicone oil, 300% hexamethylene, 431% chloroform, the i.e. sample pair
There is preferable adsorption capacity in various oil and organic reagent.
From the above content：Using polyethylene oxide and high density polyethylene (HDPE) as raw material, use is easy to operate, to environment without
When the melting extrusion method of pollution prepares high density polyethylene (HDPE) water-oil separating material, the matter of polyethylene oxide and high density polyethylene (HDPE)
Amount is than being 1:The high density polyethylene (HDPE) water-oil separating material prepared when 1 is the continuous alkene fibre bundle of high-density polyethylene, is showed continuous
Porous structure, to it is a variety of oil and organic reagents have preferable suction-operated.There is rope form using product prepared by this method
Three-dimensional porous structure, softness is continuous, can weave, and as shown in Figure 10, this method not only realizes continuous large-scale production, can make
Realize the large-scale production and application of the product with simple preparation method, braided fabric can be used as administer Crude Oil at Sea leakage and
Purify the ideal material of oil-containing sanitary sewage.
Embodiment 6
With polyethylene oxide and high density polyethylene (HDPE) mass ratio for 1:The high density polyethylene (HDPE) water-oil separating material of 1 preparation
A --- the performance detection of hdpe fiber beam sample has following steps：
（1）Soybean oil is adsorbed using the hdpe fiber beam of preparation, completes absorption later again with centrifuge to suction
Sample after oil carries out centrifugal treating, sloughs the waste oil adsorbed in sample, and waste oil is collected；
（2）Using step（1）Hdpe fiber Shu Zaici after centrifugal treating adsorbs soybean oil, that is, repeats benefit
With hdpe fiber beam；It completes to carry out centrifugal treating again after absorption, circuits sequentially use；
（3）To step（1）And step（2）After high density polyethylene (HDPE) continuous tow and centrifugal treating after middle oil suction
High density polyethylene (HDPE) continuous tow tested, as a result as shown in figure 11.
In Figure 11, square symbol horizontal line represents absorption of the high density polyethylene (HDPE) continuous tow to soybean oil in figure
Amount；Circle symbol horizontal line represents high density polyethylene (HDPE) continuous tow after oil suction and carrying out centrifugal treating, soybean in sample
The residual quantity of oil.It can be seen from the figure that high density polyethylene (HDPE) continuous tow is for soybean oil within 100 circulations
Although adsorbance some fluctuation, in the range of substantially maintaining 400 ~ 500%, and in the 100th use the sample to oil
Adsorbance remain in 400 ~ 500% adsorption range, do not significantly decrease, adsorption effect is good；After centrifugal treating
The residual quantity of soybean oil is then maintained at lower level in high density polyethylene (HDPE) continuous tow, there is 90% or more soybean oil
It is divested by centrifugal process, the residual quantity at the 100th time is still seldom, i.e., the high density using the method for the present invention preparation is poly-
Ethylene continuous tow has good repeated recycling utilize effect, while also achieving the recycling and reusing of waste oil.
Claims (7)
1. a kind of preparation method of high density polyethylene (HDPE) water-oil separating material, which is characterized in that include the following steps：
（1）Polyethylene oxide powder and deionized water are mixed to form paste, mixture is then placed in drying in baking oven until
Its quality is no longer changed, and polyethylene oxide pellet is broken for after being cooled to room temperature；
The drying temperature of the oven drying is 30 ~ 40 DEG C, drying time is 2 ~ 3 days；The broken obtained polycyclic oxygen second
The partial size of alkane pellet is 0.8 ~ 1.2mm；
（2）By step（1）Obtained in polyethylene oxide pellet and pellets of high density polyethylene be added to melt in extruder and squeeze
Continuous rope form material strip is obtained out；Wherein mass fraction shared by polyethylene oxide is 50%；
（3）By step（2）The continuous rope form material strip of melting extrusion is collected under tensionless winkler foundation state with coiling machine, and will be received
The continuous rope form material strip collected is cut into the continuous material strip of segment；
（4）By step（3）The continuous material strip of obtained segment is ultrasonically treated using deionized water at normal temperature, and leaching removes water
The polyethylene oxide of dissolubility, until the quality of the continuous material strip of segment is no longer changed；
（5）By step（4）Obtained in the continuous material strip of segment after leaching be placed in refrigerator and freeze, freezed after the completion of freezing
It is dried in drying machine, obtains high density polyethylene (HDPE) water-oil separating material, detected；
Cryogenic temperature of the material strip in refrigerator is -20 ~ -15 DEG C, cooling time is 2 ~ 5 hours；It is done in freeze drier
Temperature when dry is -85 ~ -80 DEG C, vacuum degree is 0.4 ~ 1Pa, and the time of freeze-drying is 48 ~ 72 hours.
2. the preparation method of high density polyethylene (HDPE) water-oil separating material according to claim 1, which is characterized in that described poly-
The molecular weight of ethylene oxide powder is 100000 ~ 200000.
3. the preparation method of high density polyethylene (HDPE) water-oil separating material according to claim 1, which is characterized in that step
（1）When the polyethylene oxide powder is mixed with deionized water, the mass fraction of polyethylene oxide is 40 ~ 50%.
4. the preparation method of high density polyethylene (HDPE) water-oil separating material according to claim 1, which is characterized in that described
High density polyethylene (HDPE) water-oil separating material is high density polyethylene (HDPE) continuous tow, the high density polyethylene (HDPE) continuous tow
The hole for being 1 μm to 20 μm with diameter.
5. the preparation method of high density polyethylene (HDPE) water-oil separating material according to claim 1, which is characterized in that step
（2）The extruder is Minitype twin-screw extrusion machine；The raw material in an extruder melting extrusion when, the temperature of melting extrusion
Revolving speed for 140 ~ 160 DEG C, extruder screw is 8 ~ 12rpm；Step（3）The coiling machine when being collected, coiling machine
Collecting rate is 20 ± 2cm/min.
6. a kind of high density polyethylene (HDPE) water-oil separating material using the preparation of preparation method described in claim 1 is in water-oil separating
Application.
7. a kind of high density polyethylene (HDPE) water-oil separating material, which is characterized in that the high density polyethylene (HDPE) water-oil separating material
It is to be made by preparation method described in any one of claim 1 ~ 5.
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