CN106065043A - A kind of preparation method of the Organic fluoride hydrophobic type chain extender containing ionic liquid - Google Patents
A kind of preparation method of the Organic fluoride hydrophobic type chain extender containing ionic liquid Download PDFInfo
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- CN106065043A CN106065043A CN201610598534.8A CN201610598534A CN106065043A CN 106065043 A CN106065043 A CN 106065043A CN 201610598534 A CN201610598534 A CN 201610598534A CN 106065043 A CN106065043 A CN 106065043A
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- chain extender
- type chain
- organic fluoride
- preparation
- hydrophobic type
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/69—Polymers of conjugated dienes
- C08G18/696—Polymers of conjugated dienes containing heteroatoms other than oxygen and other than the heteroatoms of copolymerised vinyl monomers
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The preparation method of a kind of Organic fluoride hydrophobic type chain extender containing ionic liquid: styrene, 1 vinyl 3 ethyl imidazol(e) hexafluorophosphoric acid salting liquid, 1 vinyl 3 butyl imidazole tetrafluoro boric acid salting liquid, 6,6,7,7,8,8,8 seven fluorine 5,5 pairs of (trifluoromethyls) 1,3 octadienes, 159 cyclodoecatrienes participate in polymerization, obtain promoting the Organic fluoride hydrophobic type chain extender of polyurethane products mechanical property and hydrophobic ability.
Description
Technical field
The present invention relates to the preparation method of a kind of chain extender, especially a kind of Organic fluoride hydrophobic type chain extender containing ionic liquid
Preparation method.
Background technology
Polyurethane material can be applicable to the every field such as coating, adhesive, rubber, synthetic material.The wherein poly-ammonia of hydrophobicity
Multiple fields such as ester material has the characteristic of its uniqueness, in insulation, bonds, waterproof, fire-retardant play extremely important effect.With
The development of science and technology and economic continuous progressive, every field for hydrophobic polyurethane material every physicochemical property want
Ask and also improving constantly, therefore, research and develop a kind of chain extender that can improve hydrophobic polyurethane material property and be extremely necessary.
CN 105131807A discloses a kind of hydrophobic aqueous fluorescent polyurethane coating and preparation method thereof, relates to fluorescence
Material and preparation method thereof.Hydrophobic aqueous fluorescent polyurethane coating is clear aqueous fluorescent type polyaminoester emulsion, by polyurethane
Mutually with inorganic fluorescent quantum dot phase composition.By the method for self-emulsifying, select diisocyanate, dihydroxylic alcohols, hydrophilic chain extender, silicon
It is high that oxygen alkane, fluoroacrylic resin etc. prepare transparency for raw material, the good aqueous polyurethane emulsion of hardness, then prepares with hydro-thermal method
Obtain the CdTe quantum aqueous solution of different-grain diameter, by polyaminoester emulsion from different CdTe quantum solution according to different ratios
Example mixes, and obtains the aqueous polyurethane emulsion of fluorescent type, is eventually adding crosslinking agent curing of coating, must have high-performance coating performance
Aqueous fluorescent type polyurethane coating.By adding the percentage of quantum dot to the design of polyurethane and regulation, obtain a series of
Drying time is short, and hydrophobic performance is excellent, and hardness is high, the fluorescent paint strong to the caking property of substrate.
CN 105473680A discloses a kind of polyurethane binder containing isocyanate component A and polyol component B,
Wherein isocyanate component A contains at least one diisocyanate or polyisocyanates and polyol component B contains following material
The alkoxylated polymerization product of mixture: castor oil or castor oil acid (i), aromatic diol or polyalcohol (ii), and there is aliphatic series
The hydroxyl of bonding and OH functional compound (iii) that OH degree of functionality is 1 to 8, and it is optionally selected from the change of the cyclic anhydride of dicarboxylic acids
Compound (iv), and it is optionally selected from the compound (v) of ring-type monoesters or diester.The invention still further relates to a kind of use that the present invention's is poly-
Urethane adhesive carries out the method for adhesive bond, a kind of element using described polyurethane binder to combine with adhesion and institute
State purposes in the construction of wind turbine for the element.
The polyurethane chain extender of prior art can the hydrophobic property of lifting polyurethane products by a relatively large margin, but also have life
Producing operating procedure complicated, for coating mechanical property, surface strength promotes unconspicuous shortcoming.
Content of the invention
Present invention aim at solving above-mentioned technical problem present in prior art, a kind of organic containing ionic liquid is provided
The preparation method of fluorine hydrophobic type chain extender.It is characterized in that preparation process includes:
By weight, 100-200 part water, 100 parts of styrene, 30-50 part 1-vinyl-3-ethyl miaow are added in a kettle.
Azoles hexafluorophosphoric acid salting liquid (mass concentration 20%), (quality is dense for 30-50 part 1-vinyl-3-butyl imidazole tetrafluoro boric acid salting liquid
Degree 20%), 5-10 part 6,6,7,7,8,8,8-seven fluoro-5, double (trifluoromethyl)-1 of 5-, 3-octadiene, 0.5-2 part 15 9-ring ten
Two carbon triolefins, 0.5-2 part benzoyl peroxide, stir, at a temperature of 80-120 DEG C, react 8-12h, reaction removes after terminating
Remove unreacted reactant, product is filtered, dry, obtain Organic fluoride hydrophobic type chain extender.
Described 1-vinyl-3-butyl imidazole tetrafluoroborate, 1-vinyl-3-ethyl imidazol(e) hexafluorophosphate is city
Sell product, the product producing such as Kate's science, industry and trade Co., Ltd of section in Lanzhou；Double (the trifluoro of the fluoro-5,5-of 6,6,7,7,8,8,8-seven
Methyl)-1,3-octadiene, 15 9-cyclodoecatrienes are commercially available prod, the product producing such as Hubei Bang Sheng Chemical Co., Ltd.
Product；Benzoyl peroxide is commercially available prod, the product producing such as Hubei Ju Sheng Science and Technology Ltd..
The product of the present invention has the advantages that
(1) this chain extender contains hydrophobic group, apply the polyurethane products of this chain extender production to have good dredging
Aqueous energy.
(2) introduce fluorine functional group, substantially increase the draftability of the polyurethane products of production, heat-resisting quantity, hardness etc.
Every mechanical property.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
In 1000L reactor, add water 150Kg, styrene 100Kg, 1-vinyl-3-ethyl imidazol(e) hexafluorophosphoric acid salting liquid
(mass concentration 20%) 40Kg, 1-vinyl-3-butyl imidazole tetrafluoro boric acid salting liquid (mass concentration 20%) 40Kg, 6,6,7,7,
Double (trifluoromethyl)-1 of 8,8,8-seven fluoro-5,5-, 3-octadiene 8Kg, 15 9-cyclodoecatriene 1Kg, benzoyl peroxide
1Kg, reacts 10h at a temperature of 100 DEG C, and reaction removes unreacted reactant after terminating, and filters product, dries, is had
Machine fluorine hydrophobic type chain extender.Products obtained therefrom numbering M-1.
Embodiment 2
In 1000L reactor, add water 150Kg, styrene 100Kg, 1-vinyl-3-ethyl imidazol(e) hexafluorophosphoric acid salting liquid
(mass concentration 20%) 30Kg, 1-vinyl-3-butyl imidazole tetrafluoro boric acid salting liquid (mass concentration 20%) 30Kg, 6,6,7,7,
Double (trifluoromethyl)-1 of 8,8,8-seven fluoro-5,5-, 3-octadiene 5Kg, 15 9-cyclodoecatriene 0.5Kg, benzoyl peroxide first
Acyl 0.5Kg, reacts 8h at a temperature of 80 DEG C, and reaction removes unreacted reactant after terminating, and filters product, dries, obtains
Organic fluoride hydrophobic type chain extender.Products obtained therefrom numbering M-2.
Embodiment 3
In 1000L reactor, add water 150Kg, styrene 100Kg, 1-vinyl-3-ethyl imidazol(e) hexafluorophosphoric acid salting liquid
(mass concentration 20%) 50Kg, 1-vinyl-3-butyl imidazole tetrafluoro boric acid salting liquid (mass concentration 20%) 50Kg, 6,6,7,7,
Double (trifluoromethyl)-1 of 8,8,8-seven fluoro-5,5-, 3-octadiene 10Kg, 15 9-cyclodoecatriene 2Kg, benzoyl peroxide
2Kg, reacts 12h at a temperature of 120 DEG C, and reaction removes unreacted reactant after terminating, and filters product, dries, is had
Machine fluorine hydrophobic type chain extender.Products obtained therefrom numbering M-3.
Comparative example 1
Being added without 6, double (trifluoromethyl)-1 of 6,7,7,8,8,8-seven fluoro-5,5-, 3-octadiene, other are with embodiment 1.Gained produces
Product numbering M-4.
Comparative example 2
Being added without 15 9-cyclodoecatrienes, other are with embodiment 1.Products obtained therefrom numbering M-5.
By weight, the chain extender of 200 parts of embodiments 1-3 and comparative example 1-3 joins the PPG of 40 parts
(PPG) with 40 parts of methyl diphenylene diisocyanates (MDI), being warming up to 100 DEG C, stirring, reaction adds 100 parts after terminating
Water, stirring, dispersion, obtain aqueous polyurethane product.Measure the contact angle of itself and water and measure paint by GB/T 1732-1993
Film-strength.It is shown in Table 1；
Table 1: the contact angle of polyurethane aqueous dispersion made by the test specimen chain extender that different process is made and heat endurance compares
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.It any with the present invention is
Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent replaces
Change or modification etc., be all covered by among protection scope of the present invention.
Claims (2)
1. the preparation method of the Organic fluoride hydrophobic type chain extender containing ionic liquid, it is characterised in that comprise the following steps:
By weight, 100-200 part water, 100 parts of styrene, 30-50 part 1-vinyl-3-ethyl miaow are added in a kettle.
Azoles hexafluorophosphoric acid salting liquid, 30-50 part 1-vinyl-3-butyl imidazole tetrafluoro boric acid salting liquid, 6,6,7,7,8,8,8-seven is fluoro-
5,5-double (trifluoromethyl)-1,3-octadiene, 0.5-2 part 15 9-cyclodoecatriene, 0.5-2 part benzoyl peroxide, stirs
Mix uniformly, at a temperature of 80-120 DEG C, react 8-12h, product is filtered, dry, obtain Organic fluoride hydrophobic type chain extender.
2. the preparation method of the Organic fluoride hydrophobic type chain extender containing ionic liquid according to claim 1, it is characterised in that: make
Double (the trifluoromethyl)-1,3-octadiene parts by weight of the fluoro-5,5-of 6,6,7,7,8,8,8-seven be 5-10 part.
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| CN201610598534.8A CN106065043B (en) | 2016-07-28 | 2016-07-28 | A kind of preparation method of the Organic fluoride hydrophobic type chain extender containing ionic liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003293A (en) * | 2017-11-15 | 2018-05-08 | 孝感市锐思新材科技有限公司 | A kind of preparation method of the chain-expanding agent new material of load |
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| CN101157739A (en) * | 2006-10-08 | 2008-04-09 | 周小雯 | Method for preparing macromolecule material chain extender |
| CN101440141A (en) * | 2007-11-23 | 2009-05-27 | 佛山市顺德区汉达精密电子科技有限公司 | Compatibilization chain extender for recycling engineering plastics |
| CN102344564A (en) * | 2011-07-15 | 2012-02-08 | 张家港柴能生物科技有限公司 | Chain extender for polyamide preparation through chain extending |
| CN102936307A (en) * | 2012-11-27 | 2013-02-20 | 山西省化工研究所 | Epoxy functionalized chain extender, and preparation method and application thereof |
| CN103881001A (en) * | 2014-03-27 | 2014-06-25 | 杭州曦茂新材料科技有限公司 | Preparation method and application of comb-type epoxy capacity-increasing chain extender for polymer material |
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| CN101157739A (en) * | 2006-10-08 | 2008-04-09 | 周小雯 | Method for preparing macromolecule material chain extender |
| CN101440141A (en) * | 2007-11-23 | 2009-05-27 | 佛山市顺德区汉达精密电子科技有限公司 | Compatibilization chain extender for recycling engineering plastics |
| CN102344564A (en) * | 2011-07-15 | 2012-02-08 | 张家港柴能生物科技有限公司 | Chain extender for polyamide preparation through chain extending |
| CN102936307A (en) * | 2012-11-27 | 2013-02-20 | 山西省化工研究所 | Epoxy functionalized chain extender, and preparation method and application thereof |
| CN103881001A (en) * | 2014-03-27 | 2014-06-25 | 杭州曦茂新材料科技有限公司 | Preparation method and application of comb-type epoxy capacity-increasing chain extender for polymer material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003293A (en) * | 2017-11-15 | 2018-05-08 | 孝感市锐思新材科技有限公司 | A kind of preparation method of the chain-expanding agent new material of load |
| CN108003293B (en) * | 2017-11-15 | 2020-12-08 | 浙江蓝域智能科技有限公司 | Preparation method of novel loaded compatibilization chain extender material |
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| CN106065043B (en) | 2018-09-18 |
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Address after: Binwang zipper street 322000 Yiwu city in Zhejiang province Jinhua city 5 District No. 3 room 602 Applicant after: Wang Jinming Address before: 315042 Zhejiang province Jiangdong District of Ningbo City Road 265 Lane 17 No. 104 Min'an room Applicant before: Wang Jinming |
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Effective date of registration: 20220712 Address after: Room 301, No. 79-80, Lane 666, Xianing Road, Jinshan District, Shanghai 201500 Patentee after: SHANGHAI LANPOLY POLYMER TECHNOLOGY Co.,Ltd. Address before: 322000 Room 602, No. 3, 5 District, Binwang Zipper Street, Yiwu City, Jinhua City, Zhejiang Province Patentee before: Wang Jinming |
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