CN106118030B - A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof - Google Patents
A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof Download PDFInfo
- Publication number
- CN106118030B CN106118030B CN201610447957.XA CN201610447957A CN106118030B CN 106118030 B CN106118030 B CN 106118030B CN 201610447957 A CN201610447957 A CN 201610447957A CN 106118030 B CN106118030 B CN 106118030B
- Authority
- CN
- China
- Prior art keywords
- porous composite
- absorption material
- oil absorption
- composite oxide
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2293—Oxides; Hydroxides of metals of nickel
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
The present invention provides a kind of porous composite oxide/polyurethane oil absorption materials and preparation method thereof, modified by the surface hydrophobicity of the preparation of classifying porous composite oxides, classifying porous composite oxides, and then obtain porous composite oxide/polyurethane oil absorption material;The oil absorption material includes polyaminoester microball and classifying porous composite oxides;Polyaminoester microball is polymerized by the pure and mild isophorone diisocyanate of polyether polyols;Classifying porous composite oxides are bivalent metal oxide MO and Al2O3Or bivalent metal oxide mixture and Al2O3It is combined;Classifying porous composite oxides and the mass ratio of hollow polyurethane foam are 1:100~5:100.The oil suction multiplying power and protect oil performance for improving oil absorption material administer field in water-oil separating and oily pollution and have important application value.The oil absorption material improves the oil suction multiplying power and protect oil performance of oil absorption material, administers field in water-oil separating and oily pollution and has important application value.
Description
Technical field
The invention belongs to functional polymer material fields, more particularly, to a kind of porous composite oxide/polyurethane oil suction
Material and preparation method thereof.
Background technique
As the important energy and the raw material of industry, oils is the indispensable production of the mankind and daily necessities, especially
The petroleum of the title of the blood vessels of industrial development.In recent years, with the utilization of continually developing of petroleum resources, marine oil overflow accident it is frequent
Occur, very big pollution is caused to ecological environment, causes the concern that people pollute oil leak event and oily waste water, oily waste water
Separation has become the research hotspot of environment chemical engineering field.
The method of processing oily waste water mainly has the methods of absorption, extraction, solidification, biodegrade, burning and oil barrier interception.
Due to simple process, processing convenience, strong operability, it is low in cost the advantages that, absorption process processing oily waste water by extensive
Concern.High oil-absorbent material is a kind of new function material different from traditional oil absorption material, has oil suction multiplying power height, grease selection
Property good and reusable equal excellent properties, therefore the exploitation of high oil-absorbent material also results in the extensive of researchers at home and abroad
Concern.
Currently, high oil-absorbent material can be divided into following three classes according to its oil-absorbing process: (1) fibrous oil absorption material utilizes fibre
The adsorption of oil absorption material and the capillarity of fibre gap and lumen are tieed up, oil product is carried out separation and recycling;(2) more
Hole oil absorption material, the main porous structure using such as mandruka, graphene aerogel, clay material, simultaneously by oil product absorption
It is stored in its duct;(3) it is swollen oil absorption material, using the stretching, extension of high molecular material reticular structure by oil product storage in high score
Sub- material internal.There is mutual affinity interaction in high molecular material between lipophilic group and oil molecule, this is the power for being swollen oil suction.
All there are many deficiencies for existing oil absorption material, such as fibrous oil absorption material and porous oil-absorbing material Oil keeping is poor, reusing
Difference, polymer oil absorption material have good Oil keeping, but there is a problem of that oil suction multiplying power is low and swelling rate is slow.
Summary of the invention
For the above deficiency exists in the prior art, the present invention provides a kind of porous composite oxide/polyurethane oil suctions
Material and preparation method thereof, by playing the oil absorption of porous material and fibrous material in conjunction with high molecular material swelling behavior
Come, improve the oil suction multiplying power and protect oil performance of oil absorption material, administering field in water-oil separating and oily pollution has important answer
With value.
The present invention achieves the above technical objects by the following technical means.
A kind of porous composite oxide/polyurethane oil absorption material, including polyaminoester microball and classifying porous composite oxides;
The polyaminoester microball is polymerized by the pure and mild isophorone diisocyanate of polyether polyols;The classifying porous composite oxides
For bivalent metal oxide MO and Al2O3Or bivalent metal oxide mixture and Al2O3It is combined;It is described classifying porous multiple
The mass ratio for closing oxide and hollow polyurethane foam is 1:100~5:100.
Preferably, the mass ratio of the pure and mild isophorone diisocyanate of the polyether polyols is 10:3~10:1;Described point
The molar ratio of Al3+ and M2+ is 1:3~1:1 in grade porous composite oxide.
Preferably, the bivalent metal oxide MO includes one of ZnO, NiO and MgO.
A kind of preparation method of porous composite oxide/polyurethane oil absorption material, includes the following steps:
S1: the preparation of classifying porous composite oxides:
At room temperature, the soluble inorganic salt, aluminium oxide and urea of metal M are added in ptfe autoclave, are mixed
It closes uniformly, in 80~140 DEG C of hydro-thermal reactions 12 of temperature~for 24 hours, successively wash, dries through cooling, filtering, distilled water and ethyl alcohol
Afterwards, in 500~800 DEG C of 2~6h of roasting of temperature, classification porous composite oxide is obtained;
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, classifying porous composite oxides described in silane coupling agent, distilled water, ethyl alcohol and step S1 are added anti-
It answers in container, after 30~60min of ultrasound, is transferred to 50~100min of processing in microwave chemical reactor, after reaction distilled water
Washing, obtains the classifying porous composite oxides of surface hydrophobicity;
S3: porous composite oxide/polyurethane oil absorption material preparation:
The classifying porous composite oxides of surface hydrophobicity described in polyether polyol, silicone oil, sodium bicarbonate and step S2 are added
Enter in reaction vessel, after mixing, isophorone diisocyanate is added, 10s~2min is stirred at 40~60 DEG C of temperature
Afterwards, it is transferred to 2~6h of reaction in 80~120 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Preferably, Al described in step S12O3Molar ratio with urea is 1:4~1:1, Al3+With M2+Molar ratio be 1:3
~1:1, the concentration of the soluble inorganic salt of metal M are 0.01~0.5mol/L.
Preferably, temperature dry described in step S1 is 70~100 DEG C, the time is 12~for 24 hours.
Preferably, volume ratio 1:30~1:60 of silane coupling agent described in step S2 and distilled water, ethyl alcohol and distilled water
Volume ratio be 1:2~2:1, mass ratio 1:10~3:10 of silane coupling agent and porous composite oxide;Distillation water washing 3~
6 times.
Preferably, silane coupling agent described in step S2 is the one of silane resin acceptor kh-550 and Silane coupling reagent KH-570
Kind or two kinds of combinations.
Preferably, polyether polyol described in step S3 and isophorone diisocyanate mass ratio are 10:3~10:1,
Silicone oil and sodium bicarbonate mass ratio are 1:2~1:1, and polyether polyol and sodium bicarbonate mass ratio are 5:1~15:1, sodium bicarbonate
Mass ratio with the classifying porous composite oxides of surface hydrophobicity is 10:7~10:1.
Preferably, polyether polyol molecular weight is 2000~4000 in step S3.
Beneficial effects of the present invention:
(1) a kind of porous composite oxide/polyurethane oil absorption material of the present invention and preparation method thereof, surface is changed
Property classifying porous composite oxides and polyurethane oil suction foam it is compound, increase polyurethane foam swelling rate while protect
Swelling behavior and protect oil performance of the polyurethane oil absorption material in oil product have been stayed, it is made to have both porous oil-absorbing material and macromolecule suction
The advantages of light wood material, improves the oil suction multiplying power and protect oil performance of oil absorption material.
(2) present invention prepares porous composite oxide, composite oxides component and the pore structure tool of preparation using hydro-thermal method
There are adjustability, especially its pore structure that diversity is presented, there is hierarchical porous structure, macropore and meso-hole structure can be existed simultaneously.It is multiple
Porous composite oxide/polyurethane oil absorption material swelling rate can be improved in the hierarchical porous structure for closing oxide, can effectively control
Mass transport process during water-oil separating processed.
(3) porous composite oxide provided by the invention/polyurethane oil absorption material component has adjustability, by more
The optimization of hole composite oxides and polyurethane foam ratio can be improved its oil suction multiplying power, performance better than porous composite oxide and
The oil absorbency of pure polyurethane foam.
(4) compared with the polyurethane foam of conventional method synthesis, porous composite oxide provided by the invention/polyurethane is inhaled
Light wood material can reach 30mg/g or more to the oil suction multiplying power of chloroform and carbon tetrachloride, and can reach absorption within a hour
Balance.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
Embodiment 1:
S1: the preparation of classifying porous composite oxides:
At room temperature, 2mmol aluminium oxide, 4mmol urea, 4mmol magnesium nitrate and 50mL distilled water are sequentially added into reaction kettle
In, it after mixing, being transferred in baking oven, 110 DEG C of reaction 12h, distilled water and ethanol washing 5 times are used in cooling, filtering respectively,
For 24 hours, 600 DEG C of roasting 4h obtain Mg-Al composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
It 70 DEG C of reaction temperature, distills water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.4g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing, after stirring 30s rapidly at 50 DEG C, transfer
Into baking oven, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 2:
S1: the preparation of classifying porous composite oxides:
At room temperature, reaction kettle is successively added in 2mmol aluminium oxide, 4mmol urea, 4mmol zinc nitrate and 50mL distilled water
In, it after mixing, is transferred in baking oven, 90 DEG C of reaction 12h, cooling, filtering, uses distilled water and ethanol washing 5 times respectively, 80
It is DEG C dry for 24 hours, 600 DEG C of roasting 4h acquisition Zn Al composite oxides.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 550,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
It 70 DEG C of reaction temperature, distills water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.4g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 30s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 3:
S1: the preparation of classifying porous composite oxides:
At room temperature, reaction kettle is successively added in 2mmol aluminium oxide, 4mmol urea, 4mmol nickel sulfate and 50mL distilled water
In, it after mixing, being transferred in baking oven, 140 DEG C of reaction 12h, distilled water and ethanol washing 5 times are used in cooling, filtering respectively,
For 24 hours, 600 DEG C of roasting 4h obtain nickel aluminium composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
It 70 DEG C of reaction temperature, distills water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.4g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 30s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 4:
S1: the preparation of classifying porous composite oxides:
At room temperature, reaction kettle is successively added in 2mmol aluminium oxide, 4mmol urea, 4mmol magnesium sulfate and 50mL distilled water
In, it after mixing, being transferred in baking oven, 120 DEG C of reaction 12h, distilled water and ethanol washing 5 times are used in cooling, filtering respectively,
For 24 hours, 600 DEG C of roasting 4h obtain Mg-Al composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
70 DEG C of reaction temperature is distilled water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.4g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 30s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 5:
S1: the preparation of classifying porous composite oxides:
At room temperature, reaction kettle is successively added in 2mmol aluminium oxide, 4mmol urea, 4mmol zinc chloride and 50mL distilled water
In, it after mixing, being transferred in baking oven, 120 DEG C of reaction 12h, distilled water and ethanol washing 5 times are used in cooling, filtering respectively,
For 24 hours, 600 DEG C of roasting 4h obtain Zn Al composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
It 70 DEG C of reaction temperature, distills water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.4g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 30s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 6:
S1: the preparation of classifying porous composite oxides:
At room temperature, 2mmol aluminium oxide, 6mmol urea, 2mmol magnesium chloride, 2mmol zinc chloride and 50mL distilled water is first
Be added in reaction kettle, after mixing, be transferred in baking oven, 120 DEG C of reaction 12h afterwards, cooling, filtering, respectively with distilled water with
Ethanol washing 5 times, for 24 hours, 600 DEG C of roasting 4h obtain Zn Al composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
It 70 DEG C of reaction temperature, distills water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.3g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 20s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
Embodiment 7:
S1: the preparation of classifying porous composite oxides:
At room temperature, 2mmol aluminium oxide, 4mmol urea, 4mmol magnesium nitrate, 2mmol nickel chloride and 50mL distilled water is first
Be added in reaction kettle, after mixing, be transferred in baking oven, 140 DEG C of reaction 12h afterwards, cooling, filtering, respectively with distilled water with
Ethanol washing 5 times, for 24 hours, 600 DEG C of roasting 4h obtain Zn Al composite oxide for 80 DEG C of dryings.
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, 1mL is taken into silane coupling agent KH 570,40mL distilled water, 40mL ethyl alcohol and 5g Mg-Al composite oxide
It is transferred in flask, after being ultrasonically treated 30min, is transferred in microwave chemical reactor, microwave treatment 60min, microwave power 700w,
70 DEG C of reaction temperature is distilled water washing 5 times after reaction, obtains the classifying porous composite oxides of surface hydrophobicity.
S3: porous composite oxide/polyurethane oil absorption material preparation:
By 10g polyether polyol, 1g sodium bicarbonate and 0.65g silicone oil and the classifying porous composite oxides of 0.1g surface hydrophobicity
It is added in reactor, 2.22g isophorone diisocyanate is added after mixing and is transferred to baking oven after stirring 20s at 50 DEG C
In, 3h is reacted in 100 DEG C of environment, obtains porous composite oxide/polyurethane oil absorption material.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (7)
1. a kind of porous composite oxide/polyurethane oil absorption material preparation method, which comprises the steps of:
S1: the preparation of classifying porous composite oxides:
At room temperature, the soluble inorganic salt, aluminium oxide and urea of metal M are added in ptfe autoclave, mixing is equal
It is even, in 80~140 DEG C of hydro-thermal reactions 12 of temperature~for 24 hours, after successively being washed through cooling, filtering, distilled water and ethyl alcohol, being dry,
500~800 DEG C of 2~6h of roasting of temperature, obtain classification porous composite oxide;
S2: the surface hydrophobicity of classifying porous composite oxides is modified:
At room temperature, reaction is added in classifying porous composite oxides described in silane coupling agent, distilled water, ethyl alcohol and step S1 to hold
In device, after 30~60min of ultrasound, it is transferred to 50~100min of processing in microwave chemical reactor, distills water washing after reaction,
Obtain the classifying porous composite oxides of surface hydrophobicity;
S3: porous composite oxide/polyurethane oil absorption material preparation:
The classifying porous composite oxides of surface hydrophobicity described in polyether polyol, silicone oil, sodium bicarbonate and step S2 are added anti-
It answers in container, after mixing, isophorone diisocyanate is added, after stirring 10s~2min at 40~60 DEG C of temperature, turn
2~6h of reaction in 80~120 DEG C of environment is moved on to, porous composite oxide/polyurethane oil absorption material is obtained.
2. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In the molar ratio of aluminium oxide described in step S1 and urea is 1:4~1:1, Al3+With M2+Molar ratio be 1:3~1:1, metal
The concentration of the soluble inorganic salt of M is 0.01~0.5mol/L.
3. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In, dry temperature described in step S1 is 70~100 DEG C, the time is 12~for 24 hours.
4. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In, volume ratio 1:30~1:60 of silane coupling agent described in step S2 and distilled water, the volume ratio of ethyl alcohol and distilled water is 1:2
Mass ratio 1:10~3:10 of~2:1, silane coupling agent and classifying porous composite oxides;Distillation water washing 3~6 times.
5. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In silane coupling agent described in step S2 is one or two kinds of groups of silane resin acceptor kh-550 and Silane coupling reagent KH-570
It closes.
6. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In polyether polyol described in step S3 and isophorone diisocyanate mass ratio are 10:3~10:1, silicone oil and bicarbonate
Sodium mass ratio is 1:2~1:1, and polyether polyol and sodium bicarbonate mass ratio are 5:1~15:1, sodium bicarbonate and surface hydrophobicity point
The mass ratio of grade porous composite oxide is 10:7~10:1.
7. a kind of preparation method of porous composite oxide/polyurethane oil absorption material according to claim 1, feature exist
In polyether polyol molecular weight is 2000~4000 in step S3.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610447957.XA CN106118030B (en) | 2016-06-20 | 2016-06-20 | A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610447957.XA CN106118030B (en) | 2016-06-20 | 2016-06-20 | A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106118030A CN106118030A (en) | 2016-11-16 |
CN106118030B true CN106118030B (en) | 2019-04-02 |
Family
ID=57471143
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610447957.XA Expired - Fee Related CN106118030B (en) | 2016-06-20 | 2016-06-20 | A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106118030B (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108285516B (en) * | 2018-02-09 | 2020-08-04 | 济南大学 | Method for preparing silicon-containing polyurethane monodisperse microspheres with high yield |
CN108892766A (en) * | 2018-07-24 | 2018-11-27 | 合肥峰腾节能科技有限公司 | Foamed material is used in a kind of efficient oil leak absorption |
CN110404296B (en) * | 2019-08-02 | 2021-04-02 | 广州大学 | Super-wettability oil-water separation material and preparation method and application thereof |
CN110724248A (en) * | 2019-10-16 | 2020-01-24 | 刘景全 | Magnetic polyurethane oil absorption foam with high hydrophobicity |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5110189A (en) * | 1974-07-16 | 1976-01-27 | Toyo Tire & Rubber Co | |
CN103736442A (en) * | 2014-01-10 | 2014-04-23 | 东南大学 | Method for preparing porous alumina composite material through biological template method |
CN105669941A (en) * | 2016-01-22 | 2016-06-15 | 江苏大学 | Preparation method and application of coal-based modified polymer foaming material |
-
2016
- 2016-06-20 CN CN201610447957.XA patent/CN106118030B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5110189A (en) * | 1974-07-16 | 1976-01-27 | Toyo Tire & Rubber Co | |
CN103736442A (en) * | 2014-01-10 | 2014-04-23 | 东南大学 | Method for preparing porous alumina composite material through biological template method |
CN105669941A (en) * | 2016-01-22 | 2016-06-15 | 江苏大学 | Preparation method and application of coal-based modified polymer foaming material |
Non-Patent Citations (2)
Title |
---|
"Enhancing oil removal from water by immobilizing multi-wall carbon nanotubes on the surface of polyurethane foam";Alireza Keshavarz et.al;《 Journal of Environmental Management》;20150424;第279-286页 * |
"聚氨酯泡沫的制备及吸油性能";魏徵等;《高分子材料科学与工程》;20101130;第26卷(第11期);第118-121页 * |
Also Published As
Publication number | Publication date |
---|---|
CN106118030A (en) | 2016-11-16 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106118030B (en) | A kind of porous composite oxide/polyurethane oil absorption material and preparation method thereof | |
Wang et al. | Synthesis of calcium materials in biochar matrix as a highly stable catalyst for biodiesel production | |
Narasimhan et al. | Heterogeneous nanocatalysts for sustainable biodiesel production: A review | |
AU2020103433A4 (en) | Method for preparing magnetic biochar from kitchen garbage | |
CN100497527C (en) | Process for preparing supported solid catalyst for use in production of bio-diesel oil | |
CN104624162B (en) | A kind of method that oil absorption material is prepared by matrix modification of palm fibre | |
CN106904625B (en) | A kind of charing method of the compound intercalated montmorillonite of cellulose | |
CN109317100A (en) | A kind of room temperature pretreatment-hydro-thermal charing method preparing magnetic algae base charcoal | |
CN101245254A (en) | Method for producing biological diesel oil with carbon-based solid acid as catalyst | |
CN101249449A (en) | Novel solid body base catalyst and applications for biological diesel oil synthesizing | |
CN103242914A (en) | Method for rapidly producing biodiesel from kitchen garbage and produced biodiesel | |
CN104109550A (en) | Method and system for preparing biological oil by antibiotic bacteria residue | |
CN101249431A (en) | Novel solid body base catalyst and applications thereof in biological diesel oil synthesizing | |
CN108456328A (en) | A kind of processing method of waste plastics | |
CN101205473B (en) | Catalyzed preparation of biodiesel by calcining sodium silicate | |
CN102559374B (en) | Method for preparing biodiesel from microalgae through one-step method by utilizing supercritical methanol | |
CN107488519A (en) | A kind of method that acid-base catalysis Bio-Diesel Fuels are loaded using magnetic charcoal | |
CN107892995A (en) | A kind of method that biodiesel is produced using waste oil in kitchen waste | |
CN107118304A (en) | A kind of preparation method of kapok fiber oil absorption material | |
CN101992061B (en) | Filter medium for removing perfluorooctane sulfonate from water and preparation method thereof | |
CN101642716B (en) | Preparation method and application of alkaline earth metal glyceride catalyst | |
CN104164304B (en) | A kind of modified resin catalysis prepares the new method of biodiesel | |
CN101249450A (en) | Solid body base catalyst and applications for biological diesel oil synthesizing | |
CN107754816A (en) | A kind of utilize is alkylated the method that spent acid prepares charcoal base acid material | |
CN104877066A (en) | Synthesis method of magnesium-aluminum bi-metal oxide composite high-oil-absorption resin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190402 Termination date: 20190620 |
|
CF01 | Termination of patent right due to non-payment of annual fee |