CN103833914A - Method for preparing fluorocarbon resin emulsion with dual cross-linking structure - Google Patents
Method for preparing fluorocarbon resin emulsion with dual cross-linking structure Download PDFInfo
- Publication number
- CN103833914A CN103833914A CN201210545283.9A CN201210545283A CN103833914A CN 103833914 A CN103833914 A CN 103833914A CN 201210545283 A CN201210545283 A CN 201210545283A CN 103833914 A CN103833914 A CN 103833914A
- Authority
- CN
- China
- Prior art keywords
- fluorocarbon resin
- resin emulsion
- monomer
- preparation
- crosslinking structure
- 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
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention discloses a method for preparing a fluorocarbon resin emulsion with a dual cross-linking structure. According to the method, intramolecular cross-linking is firstly carried out in a bifunctional monomer, then a cross-linkable unsaturated monomer and a curing agent are cross linked, by using the special effect of the dual cross-linking in the same system, a C-F bond can be fixed firmly and cannot swing arbitrarily, so as to fully shield the backbone of the molecule for long, so that the water tolerance, acid resistance, alkali resistance and weather fastness of the paint film are greatly improved, the coating is prolonged in service life so as to well protect and decorate buildings, and the material and labor cost are saved.
Description
Technical field
The present invention relates to a kind of preparation method of fluorocarbon resin emulsion, particularly a kind of preparation method of the fluorocarbon resin emulsion with dual crosslinking structure.
Background technology
From the synthetic teflon resin of The Dow Chemical Co. (US) 2030 Dow Center, Abbott Road, Midland, Michigan 48640, in 1938 so far, the history of existing six more than ten years of fluorocarbon resin, resin Cultivar development is variation.Because fluorocarbon resin has excellent performance as the coating of binding agent, more and more receive domestic and international coating personage's concern.
Existing fluorine carbon emulsion is in film process; fluorine atom can be to the surface transport of paint film; and C-F key can produce swing; thereby lose the shielding effect to molecular backbone chain; paint film is greatly affected in water-fast, acidproof, alkaline-resisting and weathering resistance; thereby coating is greatly shortened on the time limit of decorating protection building, bring larger financial loss.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of the fluorocarbon resin emulsion with dual crosslinking structure, to reach the object of water-fast, acidproof, the alkaline-resisting and weathering resistance that improves paint film.
For achieving the above object, technical scheme of the present invention is as follows:
A preparation method with the fluorocarbon resin emulsion of dual crosslinking structure, present method comprises the following steps, below proportioning be all weight percentage:
(1) 1～5% emulsifying agent is dissolved in 30%～40% deionized water, the monomer to 25%～35% under whipped state carries out pre-emulsification, and pre-emulsification 20～40min, obtains pre-emulsion.
(2) in reactor, add 20%～30% deionized water and 1～5% emulsifying agent, adopt 0.05% persulphate to drip at 80～90 ℃, drip the pre-emulsion obtaining in step 1 simultaneously, the time is 3～4 hours.
(3) reaction finish rear use 25% ammoniacal liquor regulate PH be 7～9, then add 0.5～5% solidifying agent, finally use filtered through gauze discharging.
Wherein, described emulsifying agent is one or more in the reactive emulsifier of negatively charged ion or non-ionic type.
Wherein, described monomer comprises fluorinated acrylate, acrylic ester monomer and special cross-linking monomer.
Wherein, described special cross-linking monomer is the monomer that comprises bifunctional and the unsaturated monomer that contains crosslinkable functionality.
Preferably, the monomer that comprises bifunctional described in is divinylbenzene, EDIA, butylene glycol diacrylate etc.
Preferably, the unsaturated monomer that contains crosslinkable functionality described in is diacetone-acryloamide(DAA) or methacrylic acid etheric acid ethoxylated ester etc.
Wherein, described persulphate is water miscible Potassium Persulphate, Sodium Persulfate or ammonium persulphate.
Wherein, described solidifying agent is the amine curing agents such as adipic dihydrazide, succinic acid hydrazide ii or triethylene tetramine.
Pass through technique scheme, the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure provided by the invention, first carry out intramolecular crosslinked with the monomer of bifunctional, then form crosslinked with crosslinkable unsaturated monomer and solidifying agent, utilize this dual special-effect reaching that is cross-linked in same system, can firmly C-F key be fixed, it can not be swung arbitrarily, thereby can play lasting comprehensively shielding effect to molecular backbone chain, greatly improve the water-fast of paint film, acidproof, alkaline-resisting and weathering resistance, coating is extended greatly to the decoration protection time limit of building, material and cost of labor are saved.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described.
Embodiment mono-:
(1) 1% alkyl vinyl sodium sulfonate is dissolved in 30% deionized water, mixture to 35% fluorinated acrylate, acrylic ester monomer, divinylbenzene and diacetone-acryloamide(DAA) under whipped state carries out pre-emulsification, in this mixture, the ratio of each component is 1: 1: 1: 1, pre-emulsification 20min, obtains pre-emulsion.
(2) in reactor, add 30% deionized water and 2% emulsifying agent, adopt 0.05% Ammonium Persulfate 98.5 to drip at 80 ℃, drip the pre-emulsion obtaining in step 1 simultaneously, the time is 3 hours.
(3) reaction finish rear use 25% ammoniacal liquor regulate PH be 7～9, then add 1.95% triethylene tetramine, finally use filtered through gauze discharging.
Embodiment bis-:
(1) 3% alkyl vinyl sodium sulfonate is dissolved in 35% deionized water, mixture to 25% fluorinated acrylate, acrylic ester monomer, EDIA and diacetone-acryloamide(DAA) under whipped state carries out pre-emulsification, in this mixture, the ratio of each component is 1: 1: 1: 1, pre-emulsification 30min, obtains pre-emulsion.
(2) in reactor, add 25% deionized water and 1% emulsifying agent, adopt 0.05% Potassium Persulphate to drip at 90 ℃, drip the pre-emulsion obtaining in step 1 simultaneously, the time is 4 hours.
(3) reaction finish rear use 25% ammoniacal liquor regulate PH be 7～9, then add 0.95% adipic dihydrazide, finally use filtered through gauze discharging.
The fluorocarbon resin emulsion dispersion of embodiment bis-is very even, exist without precipitation and block, and coating dispersion process can be controlled and not produce bubble, paint brush is coated with after preparation film forming, be 10 hours set time, coating adhesion reaches 0 grade, and salt water resistance performance reaches 300 days and do not ftracture, comes off, bubbles, and acid-proof alkaline reaches 10 days.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple modification of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a preparation method with the fluorocarbon resin emulsion of dual crosslinking structure, is characterized in that, present method comprises the following steps, below proportioning be all weight percentage:
(1) 1～5% emulsifying agent is dissolved in 30%～40% deionized water, the monomer to 25%～35% under whipped state carries out pre-emulsification, and pre-emulsification 20～40min, obtains pre-emulsion.
(2) in reactor, add 20%～30% deionized water and 1～5% emulsifying agent, adopt 0.05% persulphate to drip at 80～90 ℃, drip the pre-emulsion obtaining in step 1 simultaneously, the time is 3～4 hours.
(3) reaction finish rear use 25% ammoniacal liquor regulate PH be 7～9, then add 0.5～5% solidifying agent, finally use filtered through gauze discharging.
2. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 1, is characterized in that, described emulsifying agent is one or more in the reactive emulsifier of negatively charged ion or non-ionic type.
3. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 1, is characterized in that, described monomer comprises fluorinated acrylate, acrylic ester monomer and special cross-linking monomer.
4. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 3, is characterized in that, described special cross-linking monomer is the monomer that comprises bifunctional and the unsaturated monomer that contains crosslinkable functionality.
5. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 4, is characterized in that, described in comprise bifunctional monomer be divinylbenzene, EDIA or butylene glycol diacrylate etc.
6. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 4, is characterized in that, described in contain crosslinkable functionality unsaturated monomer be diacetone-acryloamide(DAA) or methacrylic acid etheric acid ethoxylated ester etc.
7. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 1, is characterized in that, described persulphate is water miscible Potassium Persulphate, Sodium Persulfate or ammonium persulphate.
8. the preparation method of the fluorocarbon resin emulsion with dual crosslinking structure according to claim 1, is characterized in that, described solidifying agent is the amine curing agents such as adipic dihydrazide, succinic acid hydrazide ii or triethylene tetramine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545283.9A CN103833914A (en) | 2012-12-17 | 2012-12-17 | Method for preparing fluorocarbon resin emulsion with dual cross-linking structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545283.9A CN103833914A (en) | 2012-12-17 | 2012-12-17 | Method for preparing fluorocarbon resin emulsion with dual cross-linking structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103833914A true CN103833914A (en) | 2014-06-04 |
Family
ID=50797838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210545283.9A Pending CN103833914A (en) | 2012-12-17 | 2012-12-17 | Method for preparing fluorocarbon resin emulsion with dual cross-linking structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103833914A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730502A (en) * | 2005-08-16 | 2006-02-08 | 广东鸿昌化工有限公司 | Microemulsion of fluorin containing crylic acid of self-crosslink in normal temperature and its production method |
| CN1896113A (en) * | 2006-06-15 | 2007-01-17 | 南开大学 | Printing fluorinated acrylic ester self-crosslinked emulsion and its preparation |
| CN102174143A (en) * | 2011-01-29 | 2011-09-07 | 锦州惠发天合化学有限公司 | Method for preparing fluorine-containing acrylate emulsion |
-
2012
- 2012-12-17 CN CN201210545283.9A patent/CN103833914A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730502A (en) * | 2005-08-16 | 2006-02-08 | 广东鸿昌化工有限公司 | Microemulsion of fluorin containing crylic acid of self-crosslink in normal temperature and its production method |
| CN1896113A (en) * | 2006-06-15 | 2007-01-17 | 南开大学 | Printing fluorinated acrylic ester self-crosslinked emulsion and its preparation |
| CN102174143A (en) * | 2011-01-29 | 2011-09-07 | 锦州惠发天合化学有限公司 | Method for preparing fluorine-containing acrylate emulsion |
Non-Patent Citations (1)
| Title |
|---|
| 严微 等: ""微波辐射制备室温自交联含氟聚丙烯酸酯乳液"", 《合成树脂及塑料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105367696A (en) | Elastic raindrop impression resisting styrene-acrylic emulsion and preparation method thereof | |
| CN103172786A (en) | Polyacrylic emulsion with good binding resistance, water resistance, smoothness and adhesive force and low-temperature film-forming property at same time | |
| CN105131866A (en) | Water-based adhesive for iron-sheet panel composite veneer and preparation method thereof | |
| CN101343525B (en) | Watersoluble adhesive agent used in imitation leather electrostatic real leather embedding product and preparation thereof | |
| CN112409877A (en) | Preparation method of flame-retardant water-based core-shell acrylate resin coating | |
| CN102321326A (en) | Acrylic ester elastic emulsion of room-temperature self crosslinking nucleocapsid structure and preparation method thereof | |
| CN105482033B (en) | A kind of polymer microballoon and its preparation method and application | |
| CN103130948A (en) | Room temperature crosslinkage and curable styrene-acrylate emulsion, and its preparation method | |
| CN103805054B (en) | A kind of concrete exterior wall protective agent and preparation method thereof | |
| CN103554378A (en) | Preparation method and application of ketoaldehyde resin modified room-temperature self-crosslinked acrylate emulsion | |
| CN101104659A (en) | Method for preparing non-soap fluorine-containing polyacrylate core-shell emulsion with crosslinking network structure | |
| CN103183491B (en) | The preparation method of crosslinking polymer cement waterproofing paint | |
| CN111363081A (en) | Acrylate emulsion for stain-resistant water-based finish varnish and preparation method thereof | |
| CN104356321A (en) | Water-based polysiloxane modified epoxy resin and preparation method thereof | |
| CN104974628A (en) | Metal roof waterproof paint and preparation method thereof | |
| CN104710575A (en) | Polyurethane-modified acrylate emulsion, preparation and application thereof in aqueous woodenware paint | |
| CN105482035B (en) | A kind of polyacrylamide and its preparation method and application | |
| CN102659976A (en) | Novel aqueous light-cured alicyclic epoxy acrylic acid emulsion and preparation method thereof | |
| CN103030735A (en) | Single-component quick air-drying water based paint resin and preparation method | |
| CN104592438A (en) | Three-layer core-shell structure interpenetrating network emulsion having high adhesion force to metal substrate and synthesis method of emulsion | |
| CN104151472A (en) | Self-crosslinking macromolecular dust suppressant and preparation method thereof | |
| CN105837739A (en) | Method for preparing water-based fluorine-containing hydroxyl acrylic emulsion | |
| CN103145906A (en) | Preparation method of environment-friendly type core-shell propyl acetate emulsion | |
| CN104017146A (en) | Water-based acrylate adhesive for reflective coatings and preparation method thereof | |
| CN106397662A (en) | Acrylic acid microgel emulsion having automatic restoration function and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| DD01 | Delivery of document by public notice |
Addressee: CHANGSHU LINRUN FLUORINE AND SILICONE MATERIAL CO., LTD. Document name: Notification of before Expiration of Request of Examination as to Substance |
|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140604 |
|
| RJ01 | Rejection of invention patent application after publication |