CN111454483A - Method for preparing hydrophobic polyurethane sponge in small amount by one-step method - Google Patents
Method for preparing hydrophobic polyurethane sponge in small amount by one-step method Download PDFInfo
- Publication number
- CN111454483A CN111454483A CN202010317374.1A CN202010317374A CN111454483A CN 111454483 A CN111454483 A CN 111454483A CN 202010317374 A CN202010317374 A CN 202010317374A CN 111454483 A CN111454483 A CN 111454483A
- Authority
- CN
- China
- Prior art keywords
- sponge
- pdms
- coating
- polydimethylsiloxane
- hydrophobic
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
Abstract
The invention discloses a method for preparing a small amount of hydrophobic polyurethane sponge by a one-step method, which comprises the following steps: firstly, cleaning polyurethane sponge; step two, preparing Polydimethylsiloxane (PDMS); step three, coating PDMS; and step four, curing the PDMS coating. The invention uses PDMS hydrophobic material to coat the polyurethane sponge fiber structure, thereby realizing hydrophobic modification simply and rapidly. The hydrophobic sponge prepared by the invention can absorb edible soybean oil with the self weight 40 times. The oil-water mixed liquid reciprocates in the hydrophobic sponge to produce a large amount of water-in-oil droplets. If the sponge is not hydrophobized, a large number of oil-in-water droplets are produced.
Description
Technical Field
The invention belongs to the field of sponge preparation, and particularly relates to a method for preparing a small amount of hydrophobic polyurethane sponge by a one-step method.
Background
The sponge is a porous material, and the internal fiber net-shaped porous structure greatly increases the contact area. The artificial polyurethane sponge has hydrophilicity, and when the sponge absorbs water, the substrate water molecules have larger contact area with the porous structure, so that the sponge has strong water absorbing capacity. Therefore, sponge materials are often used as cleaning materials for cleaning stains due to their strong absorption capacity. The cleaning work of the hydrophobic oil stain is difficult, for example, in the oil leakage event of an oil tanker, the oil stain treatment difficulty is high, so that the severe pollution of ocean water areas and even the severe damage of the ecological environment are caused. After the sponge is subjected to hydrophobic modification, the sponge has large absorption capacity, and can be used for cleaning of oil stains, and related reports indicate that the hydrophobic polyurethane sponge can absorb the oil stains which are 30-90 times of the self weight, release the oil stains through simple extrusion, and remove the oil stains again.
Polydimethylsiloxane (PDMS) is one of organic silicon, is clear and transparent in material quality, tasteless and non-toxic, acid-base resistant, high-temperature resistant, good in elasticity, good in biocompatibility and good in hydrophobic property. The Dow Corning DC184 comprises a polydimethylsiloxane precursor (liquid) and a curing agent (liquid), wherein the main chain structure of the precursor is a single bond structure formed by alternating Si and O, a side chain is methyl, the polydimethylsiloxane precursor is polymerized to form PDMS under the action of the curing agent, the PDMS can be cured after being heated, the thermoplastic property is good, and the side chain methyl endows the PDMS with stronger hydrophobic property. PDMS is therefore commonly used for hydrophobic modification of material coatings and has been reported for hydrophobic modification of sponges. The prior art of sponge material hydrophobic modification by applying PDMS mostly comprises diluting and dissolving a polydimethylsiloxane precursor and a curing agent in n-hexane or isopropanol, and then putting a sponge in the sponge to enable the polydimethylsiloxane precursor and the curing agent in the solution to have a polymerization reaction on the surface of a sponge fiber structure to form a hydrophobic surface layer. Although these processes are simplified, the roughening of the sponge material or the nano-particle coating modification are still required, and the PDMS coating process requires the support of organic reagents such as n-hexane as a solvent. However, experiments have shown that PDMS can be directly used for coating of sponge fiber structure due to its excellent adhesion and ductility, without the need for the process of roughening and finishing the sponge and diluting the PDMS.
The proportion of the polydimethylsiloxane precursor to the curing agent is mainly 10:1, and the proportion of the polydimethylsiloxane precursor to the curing agent is less than 20:1 and 5:1 in the preparation of PDMS. The preparation ratio of the precursor and the curing agent for the PDMS coating reported by the previous people is 10:1, and the PDMS prepared by a large proportion has small viscosity, good extensibility, long curing time and softness after curing, or vice versa, the 40:1 ratio has influence on the polymerization reaction and is not applicable, and the PDMS glue with the ratio of 20:1 is used for hydrophobic coating.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the defects of the prior art, the invention provides a method for preparing hydrophobic polyurethane sponge in a small amount by a one-step method. The invention mainly aims to develop a simple and rapid method for modifying polyurethane sponge by a PDMS hydrophobic coating.
The technical scheme is as follows: a one-step method for preparing a small amount of hydrophobic polyurethane sponge comprises the following steps:
step one, cleaning polyurethane sponge: cutting the sponge into 1-2cm square small pieces, ultrasonically cleaning with ultrapure water, then ultrasonically cleaning in 95-100% ethanol for 30min, and then taking out and drying at 60 ℃ for 0.5-1 h;
step two, preparing polydimethylsiloxane adhesive (PDMS): the proportion of the polydimethylsiloxane precursor to the curing agent is 20: 1; the PDMS glue used for the coating needs to be prepared fresh and mixed fully;
step three, PDMS coating: soaking the cleaned sponge small square block in freshly prepared Polydimethylsiloxane (PDMS) to ensure that the sponge is completely soaked, extruding the sponge to discharge bubbles in the sponge, and fully contacting sponge fibers with the PDMS to discharge the bubbles by a vacuum pumping method if necessary; taking out the sponge after full contact is finished, extruding Polydimethylsiloxane (PDMS) adsorbed by the sponge, and centrifuging the sponge at 2000rpm for 2 minutes in order to further remove the redundant PDMS and thin the PDMS coating;
step four, curing the PDMS coating: and (3) after the coating is finished, the PDMS on the surface of the sponge fiber is in a liquid state, and the coating is thin, so that the heating and curing are carried out by heating for 1 hour at 60 ℃, and the PDMS sponge material coating is finished.
As an optimization: and the precursor in the second step is vinyl polydimethylsiloxane.
As an optimization: and the curing agent in the second step is hydrogen-containing polydimethylsiloxane and a small amount of platinum.
Has the advantages that: the artificial polyurethane sponge has hydrophilicity, and the invention uses PDMS hydrophobic material to coat the polyurethane sponge fiber structure, thereby simply and rapidly realizing hydrophobic modification. The hydrophobic sponge prepared by the invention can absorb edible soybean oil with the self weight 40 times. The oil-water mixed liquid reciprocates in the hydrophobic sponge to produce a large amount of water-in-oil droplets. If the sponge is not hydrophobized, a large number of oil-in-water droplets are produced.
Drawings
Fig. 1 shows the contact angle of a water drop of the present invention with a hydrophobic sponge and PDMS, wherein the contact angle is 150 degrees on the left, 140 degrees on the right, and the volume of the water drop is about 5 μ l.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Examples
Step one, cleaning polyurethane sponge: cutting sponge into 1-2cm square pieces, ultrasonically cleaning with ultrapure water, ultrasonically cleaning in 95-100% ethanol for 30min, and oven drying at 60 deg.C for 0.5-1 hr;
step two, preparing Polydimethylsiloxane (PDMS): the proportion of the adopted polydimethylsiloxane precursor to the curing agent is 20:1, the glue prepared by the conventional 10:1 proportion has high viscosity and short solidification time, and the glue with the proportion of 20:1 has low viscosity, good extensibility, long solidification time and better adhesion. Therefore, a 20:1 glue is more suitable for coating. The 40:1 gel polymerization reaction was not considered to be effective. The PDMS glue used for the coating needs to be prepared fresh and mixed fully, partial polymerization reaction exists in the glue which is not prepared fresh, the viscosity of the glue is increased, and the adhesiveness is reduced;
step three, PDMS coating: soaking the cleaned sponge blocks in freshly prepared PDMS to ensure that the sponge is completely soaked, extruding the sponge to discharge bubbles in the sponge, and fully contacting the sponge fibers with the PDMS, wherein the bubbles can be discharged by a vacuum pumping method if necessary. After the contact is completed, the sponge can be taken out, PDMS adsorbed by the sponge is squeezed out, and in order to further remove redundant PDMS and thin the PDMS coating, the sponge is centrifuged at 2000rpm for 2 minutes. The viscosity of the 20:1 PDMS is relatively low, and the extensibility is good, so that the 20:1 PDMS adhesive coating is relatively thin;
step four, curing the PDMS coating: and after the coating is finished, the PDMS on the surface of the sponge fiber is liquid, and the coating is thin, so that the heating and curing are carried out for 1 hour at the temperature of 60 ℃. So far, the coating of the PDMS sponge material is completed.
When the technology is applied to perform the sponge hydrophobization treatment, the performance of the sponge is equivalent to that of PDMS, and the sponge has stronger hydrophobicity and lipophilicity. Actually, the contact angle between the water drop and the surface thereof is measured to be 150 degrees (the left graph of fig. 1), which is larger than the contact angle between the water drop and the PDMS (140 degrees, the right graph of fig. 1), which indicates that the sponge material has good hydrophobic property. The proportion of the used PDMS is 20:1, so that the adhesion property is good, the solidification time is long, the flexibility is good, the adhesion effect of the PDMS and the surface of the cleaned sponge fiber is strong, and the prepared hydrophobic sponge can be repeatedly used for many times without the phenomenon that the hydrophobic property is reduced due to the falling off of a coating. The coating thickness of PDMS is measured by microscopic imaging analysis, and the result shows that the coating is very thin, can be ignored relative to thicker sponge fiber, has no influence on the size of the internal space of the sponge, and has no influence on the absorption capacity of the sponge. The method is a PDMS one-step coating sponge hydrophobic modification method, and has the advantages of simple principle and convenient operation. However, since PDMS is not well formulated on a large scale (will set), this method is more suitable than the rapid preparation of small quantities of hydrophobic sponges.
Claims (3)
1. A method for preparing a small amount of hydrophobic polyurethane sponge by a one-step method is characterized by comprising the following steps: the method comprises the following steps:
step one, cleaning polyurethane sponge: cutting the sponge into 1-2cm square small pieces, ultrasonically cleaning with ultrapure water, then ultrasonically cleaning in 95-100% ethanol for 30min, and then taking out and drying at 60 ℃ for 0.5-1 h;
step two, preparing polydimethylsiloxane adhesive (PDMS): the proportion of the polydimethylsiloxane precursor to the curing agent is 20: 1; the PDMS glue used for the coating needs to be prepared fresh and mixed fully;
step three, PDMS coating: soaking the cleaned sponge small square block in freshly prepared Polydimethylsiloxane (PDMS) to ensure that the sponge is completely soaked, extruding the sponge to discharge bubbles in the sponge, and fully contacting sponge fibers with the PDMS to discharge the bubbles by a vacuum pumping method if necessary; taking out the sponge after full contact is finished, extruding Polydimethylsiloxane (PDMS) adsorbed by the sponge, and centrifuging the sponge at 2000rpm for 2 minutes in order to further remove the redundant PDMS and thin the PDMS coating;
step four, curing the PDMS coating: and (3) after the coating is finished, the PDMS on the surface of the sponge fiber is in a liquid state, and the coating is thin, so that the heating and curing are carried out by heating for 1 hour at 60 ℃, and the PDMS sponge material coating is finished.
2. The one-step method for preparing a small amount of hydrophobic polyurethane sponge according to claim 1, wherein: and the precursor in the second step is vinyl polydimethylsiloxane.
3. The one-step method for preparing a small amount of hydrophobic polyurethane sponge according to claim 1, wherein: and the curing agent in the second step is hydrogen-containing polydimethylsiloxane and a small amount of platinum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010317374.1A CN111454483A (en) | 2020-04-21 | 2020-04-21 | Method for preparing hydrophobic polyurethane sponge in small amount by one-step method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010317374.1A CN111454483A (en) | 2020-04-21 | 2020-04-21 | Method for preparing hydrophobic polyurethane sponge in small amount by one-step method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111454483A true CN111454483A (en) | 2020-07-28 |
Family
ID=71675542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010317374.1A Pending CN111454483A (en) | 2020-04-21 | 2020-04-21 | Method for preparing hydrophobic polyurethane sponge in small amount by one-step method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111454483A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542221A (en) * | 2015-12-18 | 2016-05-04 | 河南大学 | Wear-resistant super-hydrophobic super-lipophilic polyurethane sponge and preparation method and application thereof in oil-water continuous separation |
| CN105688846A (en) * | 2016-03-04 | 2016-06-22 | 桂林理工大学 | Method for preparing efficient oil-water separation sponge |
| CN111116978A (en) * | 2019-12-27 | 2020-05-08 | 浙江工业大学 | Super-durable hydrophobic three-dimensional porous oil-water separation sponge material and preparation method and application thereof |
-
2020
- 2020-04-21 CN CN202010317374.1A patent/CN111454483A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542221A (en) * | 2015-12-18 | 2016-05-04 | 河南大学 | Wear-resistant super-hydrophobic super-lipophilic polyurethane sponge and preparation method and application thereof in oil-water continuous separation |
| CN105688846A (en) * | 2016-03-04 | 2016-06-22 | 桂林理工大学 | Method for preparing efficient oil-water separation sponge |
| CN111116978A (en) * | 2019-12-27 | 2020-05-08 | 浙江工业大学 | Super-durable hydrophobic three-dimensional porous oil-water separation sponge material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Facile and scalable fabrication of superhydrophobic and superoleophilic PDMS-co-PMHS coating on porous substrates for highly effective oil/water separation | |
| Jia et al. | Efficiently texturing hierarchical epoxy layer for smart superhydrophobic surfaces with excellent durability and exceptional stability exposed to fire | |
| CN109012199B (en) | Anti-wetting super-hydrophobic membrane and preparation method thereof | |
| Zhu et al. | Superhydrophobic melamine–formaldehyde sponge functionalized by coupling agent–isocyanate siloxane as efficient absorbents for oil and organic solvents | |
| CN107583470A (en) | Super hydrophilic and underwater superoleophobic water-oil separationg film and preparation method thereof | |
| CN109837758B (en) | Preparation method of fabric super-hydrophobic surface | |
| CN105778149B (en) | A kind of preparation method of super hydrophobic polyurethane sponge | |
| CN107500561B (en) | Glass coating with high transparency, super-lubrication and self-supplement performance as well as preparation method and application thereof | |
| CN114058222B (en) | Dual self-repairing super-hydrophobic coating and preparation method thereof | |
| CN113698653A (en) | Hydrophilic coating based on acrylic polymerization and photocuring and preparation method thereof | |
| CN108043246B (en) | Preparation method of super-hydrophilic organic membrane based on micro-nano structure surface imprinting | |
| CN108043235A (en) | A kind of method for enhancing interfacial adhesion between organic separation membrane and backing material | |
| CN109593390A (en) | A kind of titanium dioxide with the lasting Superhydrophilic of high transparency-organic composite automatic cleaning coating and its mild preparation method | |
| CN107531933A (en) | The manufacture method of porous body and porous body | |
| CN111760469A (en) | Preparation method of tannin and gelatin hydrophilic coating film | |
| CN107903734A (en) | The preparation method of water-fast long-acting antifog frost-resistant high transparency coating with self-healing properties | |
| CN105418837B (en) | A kind of be separated causes the preparation method of porous super hydrophobic coating material | |
| CN109536006A (en) | A kind of preparation method of polysulfones super hydrophobic surface | |
| Abu Elella et al. | Superwetting cotton textiles for separation of oil/water mixtures | |
| CN104150787B (en) | A kind of Induced by Dopamine sol-gal process prepares the method for modifying of high hydrophiling coating | |
| CN109804029A (en) | Thin worm property and ice-phobic composition with liquid additive | |
| CN111454483A (en) | Method for preparing hydrophobic polyurethane sponge in small amount by one-step method | |
| CN114276720A (en) | Stable oil pollution resistant material, coating, preparation method and application thereof | |
| CN113462014A (en) | Super-hydrophobic sponge with photo-thermal effect and preparation method thereof | |
| CN1814411A (en) | Adsorption sheet for fixing polishing substrate and its manufacturing method and polishing device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200728 |