CN111334155A - Hydrophobic polyacrylate finishing agent containing POSS and preparation method thereof - Google Patents
Hydrophobic polyacrylate finishing agent containing POSS and preparation method thereof Download PDFInfo
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- CN111334155A CN111334155A CN202010311631.0A CN202010311631A CN111334155A CN 111334155 A CN111334155 A CN 111334155A CN 202010311631 A CN202010311631 A CN 202010311631A CN 111334155 A CN111334155 A CN 111334155A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C09D151/085—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds on to polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
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- Polymers & Plastics (AREA)
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Abstract
The invention relates to a preparation method of a hydrophobic polyacrylate finishing agent containing POSS, which is applied to a leather finishing process and can endow leather with good hydrophobicity and mechanical properties. The invention comprises the following steps: mixing 2.4-6.0g of methyl methacrylate and 3.6-7.2g of butyl acrylate, and adding 0.06-0.3g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment to completely disperse POSS; dissolving gDNS-86 in 30-50ml of distilled water, mixing with an oil phase, emulsifying for 5-10min, performing ultrasonic treatment to form miniemulsion, dissolving ammonium persulfate in the distilled water, pouring the miniemulsion and 10ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1-2h at 70 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3-5h, and cooling to room temperature to obtain the composite emulsion.
Description
The technical field is as follows:
the invention relates to a preparation method of emulsion, in particular to a hydrophobic polyacrylate finishing agent containing POSS and a preparation method thereof.
Background art:
leather products such as automobile seat cushions, sofa leather, clothing leather and the like are popularized in the life of people, but the problem of difficult cleaning treatment exists. The hydrophobic leather finishing agent has lower surface energy, so that the adhesion and corrosion of external dirt to leather can be effectively reduced, and the protective effect is achieved. Low surface energy fluoropolymers such as perfluoroalkyl carboxylates or perfluoroalkyl sulfonates are often used to make hydrophobic leather finishes, but fluoropolymers such as perfluoroalkyl carboxylates or perfluoroalkyl sulfonates pose the risk of releasing highly toxic substances into the environment, and the materials are expensive and difficult to degrade. Therefore, the development of the environment-friendly fluorine-free hydrophobic finishing agent has important significance.
Polyhedral oligomeric silsesquioxane (POSS) is an organic-inorganic hybrid material with a nanoscale three-dimensional structure, and has special structural characteristics and is receiving much attention. The POSS is introduced into the coating, and the rigid cage structure of the POSS can obviously improve the mechanical property of the coating; meanwhile, as a hybrid material with high silicon content, the surface energy of the coating can be reduced, and the hydrophobic property of the coating can be improved. Polyacrylate emulsion (PA) is a film forming substance which is most widely applied in leather finishing materials due to excellent film forming property, good gloss retention, excellent mechanical property and bonding property. Currently, there is no example in the prior art of the incorporation of octavinyl POSS into polyacrylate emulsions.
The invention content is as follows:
the invention aims to provide a hydrophobic polyacrylate finishing agent containing POSS and a preparation method thereof, and the hydrophobic polyacrylate finishing agent is applied to a leather finishing process and can endow leather with good hydrophobicity and mechanical properties. The method avoids the use of fluorine-containing polymer, and is a preparation method of the environment-friendly hydrophobic leather coating.
In order to achieve the purpose, the invention adopts the technical scheme that:
the hydrophobic polyacrylate finishing agent containing POSS is characterized in that: the material is prepared from octavinyl POSS0.06-0.3 weight parts, butyl acrylate 3.6-7.2 weight parts, and methyl methacrylate 2.4-6.0 weight parts.
A preparation method of a hydrophobic polyacrylate finishing agent containing POSS is characterized by comprising the following steps: the method comprises the following steps:
0.06-0.3 part by weight of octavinyl POSS, 3.6-7.2 parts by weight of butyl acrylate and 2.4-6.0 parts by weight of methyl methacrylate are adopted as polymerization monomers, and polyacrylate composite emulsion containing POSS is prepared by a miniemulsion polymerization method.
The method specifically comprises the following steps:
mixing 2.4-6.0g of methyl methacrylate and 3.6-7.2g of butyl acrylate, and adding 0.06-0.3g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 5-10min to completely disperse POSS; dissolving 0.036-0.084g of DNS-86 in 30-50ml of distilled water, mixing with an oil phase, emulsifying for 5-10min, performing ultrasonic treatment for 5-10min to form a miniemulsion, dissolving 0.54-1.0g of ammonium persulfate in 30-45ml of distilled water, pouring the miniemulsion and 10-20ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting at 70-80 ℃ for 1-2h, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3-5h, and cooling to room temperature to obtain the composite emulsion.
The specific technical scheme 1 comprises the following steps:
2.4g of methyl methacrylate and 4.0g of butyl acrylate were mixed, and 0.06g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 5min to completely disperse POSS; dissolving 0.036g of DNS-86 in 30ml of distilled water, mixing with an oil phase, emulsifying for 5min, and performing ultrasonic treatment for 5min to form miniemulsion, simultaneously dissolving 0.54g of ammonium persulfate in 30ml of distilled water, pouring the miniemulsion and 10ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3h, and cooling to room temperature to obtain the composite emulsion.
The specific technical scheme 2 comprises the following steps:
mixing 3.0g of methyl methacrylate and 4.8g of butyl acrylate, and adding 0.1g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 6min to completely disperse POSS; dissolving 0.05g of DNS-86 in 35ml of distilled water, mixing with an oil phase, emulsifying for 6min, and performing ultrasonic treatment for 6min to form miniemulsion, dissolving 0.6g of ammonium persulfate in 45ml of distilled water, pouring the miniemulsion and 12ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.2h at 72 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3.5h, and cooling to room temperature to obtain the composite emulsion.
The specific technical scheme 3 comprises the following steps:
4.0g of methyl methacrylate and 5.0g of butyl acrylate were mixed, and 0.22g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 7min to completely disperse POSS; dissolving 0.06g of DNS-86 in 38ml of distilled water, mixing with an oil phase, emulsifying for 7min, and performing ultrasonic treatment for 7min to form miniemulsion, dissolving 0.7g of ammonium persulfate in 40ml of distilled water, pouring the miniemulsion and 15ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.5h at 75 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 4h, and cooling to room temperature to obtain the composite emulsion.
Compared with the prior art, the invention has the following advantages and effects:
1. according to the invention, a miniemulsion polymerization method is adopted, and octavinyl POSS is introduced into the polyacrylate emulsion, so that the high silicon content of POSS and the rough structure formed on the surface of leather can effectively reduce the surface energy of the coated leather, endow the leather with good hydrophobicity and improve the mechanical property of the coated leather sample; the cross-linking degree of an emulsion system can be increased by the POSS multi-side chain structure, and the mechanical property of the finished leather sample is effectively improved.
2. According to the invention, POSS with high silicon content is introduced into the polyacrylic acid composite emulsion, and the POSS is applied to a leather finishing process. Compared with a leather sample coated with polyacrylate, the contact angle of the leather sample coated with the POSS polyacrylate composite emulsion is 115 degrees, and is improved by 40 degrees. The method avoids the use of fluorine-containing polymer, and is a preparation method of the environment-friendly hydrophobic leather coating.
Description of the drawings:
FIG. 1 shows the contact angles of leather samples after finishing, wherein a, b and c are respectively synthesized PA-POSS, laboratory synthesized polyacrylate and commercial polyacrylate;
FIG. 2 shows the tear strength and softness of finished leather samples, wherein samples 1, 2, and 3 are respectively a laboratory synthetic polyacrylate, a commercially available polyacrylate, and a PA-POSS composite emulsion.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to specific embodiments. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. The implementation conditions used in the examples can be further adjusted according to the specific experimental environment, and the implementation conditions not mentioned are generally the conditions in routine experiments.
The invention adopts octavinyl POSS, butyl acrylate and methyl methacrylate as polymerization monomers, and polyacrylate composite emulsion containing POSS is prepared by miniemulsion polymerization.
Example 1:
2.4g of methyl methacrylate and 4.0g of butyl acrylate were mixed, and 0.06g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 5min to completely disperse POSS; dissolving 0.036g of DNS-86 in 30ml of distilled water, mixing with an oil phase, emulsifying for 5min, and performing ultrasonic treatment for 5min to form miniemulsion, simultaneously dissolving 0.54g of ammonium persulfate in 30ml of distilled water, pouring the miniemulsion and 10ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3h, and cooling to room temperature to obtain the composite emulsion.
Example 2:
mixing 3.0g of methyl methacrylate and 4.8g of butyl acrylate, and adding 0.1g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 6min to completely disperse POSS; dissolving 0.05g of DNS-86 in 35ml of distilled water, mixing with an oil phase, emulsifying for 6min, and performing ultrasonic treatment for 6min to form miniemulsion, dissolving 0.6g of ammonium persulfate in 45ml of distilled water, pouring the miniemulsion and 12ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.2h at 72 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3.5h, and cooling to room temperature to obtain the composite emulsion.
Example 3:
4.0g of methyl methacrylate and 5.0g of butyl acrylate were mixed, and 0.22g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 7min to completely disperse POSS; dissolving 0.06g of DNS-86 in 38ml of distilled water, mixing with an oil phase, emulsifying for 7min, and performing ultrasonic treatment for 7min to form miniemulsion, dissolving 0.7g of ammonium persulfate in 40ml of distilled water, pouring the miniemulsion and 15ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.5h at 75 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 4h, and cooling to room temperature to obtain the composite emulsion.
Example 4
5.4g of methyl methacrylate and 6.0g of butyl acrylate were mixed, and 0.24g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 8min to completely disperse POSS; dissolving 0.072DNS-86 in 30ml of distilled water, mixing with an oil phase, emulsifying for 8min, and performing ultrasonic treatment for 8min to form miniemulsion, dissolving 0.8g of ammonium persulfate in 42ml of distilled water, pouring the miniemulsion and 16ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.8h at 78 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 4.5h, and cooling to room temperature to obtain the composite emulsion.
Example 5:
mixing 6.0g of methyl methacrylate and 7.2g of butyl acrylate, and adding 0.28g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 10min to completely disperse POSS; dissolving 0.08g of DNS-86 in 30ml of distilled water, mixing with an oil phase, emulsifying for 5min, performing ultrasonic treatment for 10min to form miniemulsion, dissolving 0.9g of ammonium persulfate in 45ml of distilled water, pouring the miniemulsion and 20ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 2h at 80 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 5h, and cooling to room temperature to obtain the composite emulsion.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (6)
1. The hydrophobic polyacrylate finishing agent containing POSS is characterized in that: the material is prepared from octavinyl POSS0.06-0.3 weight parts, butyl acrylate 3.6-7.2 weight parts, and methyl methacrylate 2.4-6.0 weight parts.
2. A preparation method of a hydrophobic polyacrylate finishing agent containing POSS is characterized by comprising the following steps: the method comprises the following steps:
0.06-0.3 part by weight of octavinyl POSS, 3.6-7.2 parts by weight of butyl acrylate and 2.4-6.0 parts by weight of methyl methacrylate are adopted as polymerization monomers, and polyacrylate composite emulsion containing POSS is prepared by a miniemulsion polymerization method.
3. The method for preparing the hydrophobic polyacrylate finishing agent containing POSS as claimed in claim 1, wherein the method comprises the following steps:
the method comprises the following steps:
mixing 2.4-6.0g of methyl methacrylate and 3.6-7.2g of butyl acrylate, and adding 0.06-0.3g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 5-10min to completely disperse POSS; dissolving 0.036-0.084g of DNS-86 in 30-50ml of distilled water, mixing with an oil phase, emulsifying for 5-10min, performing ultrasonic treatment for 5-10min to form a miniemulsion, dissolving 0.54-1.0g of ammonium persulfate in 30-45ml of distilled water, pouring the miniemulsion and 10-20ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting at 70-80 ℃ for 1-2h, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3-5h, and cooling to room temperature to obtain the composite emulsion.
4. The method for preparing a hydrophobic polyacrylate finishing agent containing POSS according to claim 1 or 2, wherein the method comprises the following steps:
the method comprises the following steps:
2.4g of methyl methacrylate and 4.0g of butyl acrylate were mixed, and 0.06g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 5min to completely disperse POSS; dissolving 0.036g of DNS-86 in 30ml of distilled water, mixing with an oil phase, emulsifying for 5min, and performing ultrasonic treatment for 5min to form miniemulsion, simultaneously dissolving 0.54g of ammonium persulfate in 30ml of distilled water, pouring the miniemulsion and 10ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1h at 70 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3h, and cooling to room temperature to obtain the composite emulsion.
5. The method for preparing a hydrophobic polyacrylate finishing agent containing POSS according to claim 1 or 2, wherein the method comprises the following steps:
the method comprises the following steps:
mixing 3.0g of methyl methacrylate and 4.8g of butyl acrylate, and adding 0.1g of octavinyl POSS to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 6min to completely disperse POSS; dissolving 0.05g of DNS-86 in 35ml of distilled water, mixing with an oil phase, emulsifying for 6min, and performing ultrasonic treatment for 6min to form miniemulsion, dissolving 0.6g of ammonium persulfate in 45ml of distilled water, pouring the miniemulsion and 12ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.2h at 72 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 3.5h, and cooling to room temperature to obtain the composite emulsion.
6. The method for preparing a hydrophobic polyacrylate finishing agent containing POSS according to claim 1 or 2, wherein the method comprises the following steps:
the method comprises the following steps:
4.0g of methyl methacrylate and 5.0g of butyl acrylate were mixed, and 0.22g of octavinyl POSS was added to form an oil phase mixture; placing the oil phase mixture in a cell crusher for ultrasonic treatment for 7min to completely disperse POSS; dissolving 0.06g of DNS-86 in 38ml of distilled water, mixing with an oil phase, emulsifying for 7min, and performing ultrasonic treatment for 7min to form miniemulsion, dissolving 0.7g of ammonium persulfate in 40ml of distilled water, pouring the miniemulsion and 15ml of ammonium persulfate initiator solution into a three-neck flask, stirring and reacting for 1.5h at 75 ℃, dropwise adding the rest of ammonium persulfate aqueous solution, continuing to react for 4h, and cooling to room temperature to obtain the composite emulsion.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010311631.0A CN111334155A (en) | 2020-04-20 | 2020-04-20 | Hydrophobic polyacrylate finishing agent containing POSS and preparation method thereof |
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| CN202010311631.0A CN111334155A (en) | 2020-04-20 | 2020-04-20 | Hydrophobic polyacrylate finishing agent containing POSS and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037614A (en) * | 2015-09-08 | 2015-11-11 | 陕西科技大学 | High-solid-content leather finishing agent prepared on basis of miniemulsion polymerization method and method thereof |
| CN105131780A (en) * | 2015-08-28 | 2015-12-09 | 华南理工大学 | POSS-block-containing acrylate copolymer super-hydrophobic coating and preparing method thereof |
| KR20170044964A (en) * | 2015-10-16 | 2017-04-26 | 동우 화인켐 주식회사 | Composition for forming hard coating and optical film using the same |
| CN107987387A (en) * | 2017-12-15 | 2018-05-04 | 会通新材料股份有限公司 | A kind of high modulus polypropylene/cage-type silsesquioxane micro foaming composite material and preparation method thereof |
| CN110511384A (en) * | 2018-05-21 | 2019-11-29 | 北京化工大学 | A kind of polyacrylate/polysilsesquioxane core-shell emulsion and preparation method thereof |
-
2020
- 2020-04-20 CN CN202010311631.0A patent/CN111334155A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131780A (en) * | 2015-08-28 | 2015-12-09 | 华南理工大学 | POSS-block-containing acrylate copolymer super-hydrophobic coating and preparing method thereof |
| CN105037614A (en) * | 2015-09-08 | 2015-11-11 | 陕西科技大学 | High-solid-content leather finishing agent prepared on basis of miniemulsion polymerization method and method thereof |
| KR20170044964A (en) * | 2015-10-16 | 2017-04-26 | 동우 화인켐 주식회사 | Composition for forming hard coating and optical film using the same |
| CN107987387A (en) * | 2017-12-15 | 2018-05-04 | 会通新材料股份有限公司 | A kind of high modulus polypropylene/cage-type silsesquioxane micro foaming composite material and preparation method thereof |
| CN110511384A (en) * | 2018-05-21 | 2019-11-29 | 北京化工大学 | A kind of polyacrylate/polysilsesquioxane core-shell emulsion and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张剑桥等: "乙烯基POSS-丙烯酸酯共聚乳液性能研究", 《涂料工业》 * |
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Application publication date: 20200626 |