CN105254803A - Method for preparing fluorine-containing hydrophobic and oileophobic textile finishing agent - Google Patents
Method for preparing fluorine-containing hydrophobic and oileophobic textile finishing agent Download PDFInfo
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- CN105254803A CN105254803A CN201510801376.7A CN201510801376A CN105254803A CN 105254803 A CN105254803 A CN 105254803A CN 201510801376 A CN201510801376 A CN 201510801376A CN 105254803 A CN105254803 A CN 105254803A
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Abstract
The invention provides a method for preparing a fluorine-containing hydrophobic and oileophobic textile finishing agent. The method comprises the following steps: adding a fluorine-containing monomer, methyl methacrylate, a soft monomer, methacrylic acid dimethylamino ethyl ester, a cross-linking monomer, butyl acrylate, azodiisobutyronitrile and N,N-dimethylformamide, heating, and stirring to react, thereby preparing a fluorine-containing hydrophobic and oileophobic textile finishing agent high polymer; dropping a potassium peroxodisulfate saturated solution, and continuously keeping the temperature and stirring; cooling to the room temperature, discharging the material out, dissolving the obtained polymer in an alcohol solvent, thereby obtaining the fluorine-containing hydrophobic and oileophobic textile finishing agent. The fluorine-containing hydrophobic and oileophobic textile finishing agent prepared by using the method provided by the invention is simple and convenient to operate, free of emulsifier and small in content of fluorine-containing monomer, and the product exists in a solid manner, and is convenient to store and transport and relatively good in both hydrophobic and oileophobic property.
Description
Technical field
The present invention relates to a kind of preparation method field of fluorine-containing two thin fabric finishing agent.
Background technology
Two thin material refers to have a class material that is hydrophobic, oleophobic property, and this kind of material can make the free energy of solid surface reduce, and has the characteristic of pollution-free, automatically cleaning, low frictional properties, hydrophobic, oleophobic.The surface of natural lotus leaf, Rice Leaf and insect wing all has extremely low free energy, and water and the oily surface that can not soak them, therefore study and explore the material with two thin performances, its tempting application prospect has evoked the concern of people.
Organo-fluorine polymer refers to the macromolecular material that fluorochemicals is polymerized (solution polymerization or letex polymerization) under certain condition, due to many characteristics of fluorine, it can give the character of the many uniquenesses of material surface, as the characteristic of low surface energy and low sticking power, there is preferably two thin property, weathering resistance, winter hardiness, high temperature resistant, corrosion-resistant, therefore the important events that traditional material cannot be applied are widely used in, as advanced vehicle coating, aircraft surfaces are covered with paint, lacquer, colour wash, etc.Research in the world about organo-fluorine polymer starts from the fifties, and has had industrialization product to come out in the eighties, such as 3M company, E.I.Du Pont Company, Asahi Glass company, large King Company etc.China starts late in this respect, starts from the seventies, but due to fluorine chemical basic material expensive, therefore the industrialization of product need raw materials cost reduction and find good cheap substitute.
For many years, people have carried out a large amount of research work to the waterproof oil-proof finishing of fabric.Originally, arrange fabric with organosilicon, discovery can give fabric good water-repellancy, but grease proofness is poor.Finding afterwards, and can give fabric excellent hydro-oleophobicity with carrying out process containing fluoroalkyle compound to fabric.Through the development of decades, fluorine-containing textile finishing agent commercialization occupy very large market.The development of fluorine-containing textile finishing agent, has greatly enriched the research field of organic fluorine material.Why fluorine-containing textile finishing agent can just cause the great interest of people once appearance and constantly be developed, mainly be that it has excellent performance, this is because due to the electronegativity of fluorine atom large, diameter is little, the shielding of C-C key can be got up, make it the stability with height.Very high stability is all demonstrated under the various environment such as strong acid, highly basic, high temperature and high radiation.In addition, fluorine-containing textile finishing agent has the feature of lower concentration, high effect, the feel making the fabric of process keep good, excellent ventilation property and water vapour permeability.So fluorine-containing textile finishing agent all has incomparable advantage in each side such as hydrophobic and lyophobic property, didirtresistance, washing fastness, rub resistance, erosion resistances compared with the finishing composition of other types.Thus developed rapidly, become the main flow of two thin finishing composition.
Fluorine material has low surface property, therefore, has the fluorochemicals of low surface energy effect or the film of fluoropolymer at material surface grafting last layer, becomes the most cost-effective method in the two thin material of preparation.Textile finishing is on fabric, apply a kind of finishing composition, and it can change the surface property of fabric, gives the performance that fabric face is special.If hydrophobic and oil repellent arrangement is the finishing composition process fabric with low surface energy, changes the surface property of fabric, make fabric face not easily by water or oily wetting and spreading, reach the object of hydrophobic and oil repellent.
Fluorine-contained finishing agent not only can give clothing hydrophobic oleophobic and antifouling decontaminable characteristic, and maintains the color and luster of fabric itself, comfort level as far as possible, and have the characteristic of lower concentration high effect, therefore fluorine-contained finishing agent becomes the fabric finishing agent of current main flow.Wherein acrylate containing fluorine multipolymer is on the basis keeping the good snappiness of acrylic polymer, cohesiveness, weathering resistance, give the surface property of multipolymer excellence, the grease proofing higher grade of fabric waterproof arranged with fluoro-acrylate copolymer, maintains good washing fastness.
Application number 201410356059.4 (publication date is 2014.12.10) discloses a kind of high hydrophobic oleophobic type powder coating, and it is made up of the raw material of following mass parts: Hexafluorobutyl mathacrylate 2-4, E12 epoxy resin 50-60, ultramarine 1-2, tetraethylene pentamine 4-10, Rutile type Titanium Dioxide 5-10, wetting enhancer LD-608A1-2, stannous octoate 0.6-1, phenylpropyl alcohol triazole 0.5-1, lauric acid amide of ethanol 1-2, compounded mix 5-10; The powder coating coating of this invention has the hydrophobic of excellence, and oleophobic surface characteristic, can significantly improve the contamination resistance of body surface, has excellent corrosion resistance nature and surface abrasion resistance simultaneously.Application number 201110266897.9 (publication date is 2012.05.02) discloses the preparation method on a kind of ultra-amphosphobic polymkeric substance and ultra-amphosphobic surface, first-selected to base material pre-treatment; Microballoon is placed in containing fluorous solvent, ultrasonic dissolution, obtains microballoon aaerosol solution; In microspheres solution, add ultra-amphosphobic polymkeric substance, hydrochloric acid tetrahydrofuran solution and water under stirring, then put into base material, reaction 5-24h; Base material is taken out, successively with containing fluorous solvent, methyl alcohol, water washing, then vacuum-drying, namely obtains ultra-amphosphobic surface.The ultra-amphosphobic polymkeric substance of this invention can give the good surface hydrophobicity ability of substrate and oleophobic ability; Again because the existing fluoropolymer feature of this polymkeric substance can carry out chemical bonding with substrate surface, ensure that gained ultra-amphosphobic surface has good scrubbing resistance and erosion resistance.Application number 201110090620.5 (publication date is 2011.09.28) discloses a kind of two fluorine-containing crosslinkable block copolymers of thin property and preparation method thereof and application.This segmented copolymer can be used for preparing the super two open coat of glass or printer paper surface, and it comprises the following steps: nano silicon spheres is placed in phenylfluoroform by (1), obtains nano silicon spheres solution; (2) in nano silicon spheres solution, add the two fluorine-containing crosslinkable block copolymers solution of thin property, tetrahydrofuran (THF), hydrochloric acid soln and water, react 7 ~ 12 hours, obtain modified Nano silicon ball crude product; (3) wash modified Nano silicon ball crude product, obtain modified Nano silicon ball; (4) modified Nano silicon ball is distributed in phenylfluoroform, wiring solution-forming; Solution is added drop-wise on sheet glass, after solvent evaporates, forms super two coating of dredging in glass sheet surface; Or immersed by printer paper in solution, take out the scraps of paper and form super two open coat on its surface after scraps of paper drying, its final material prepared is solution, is inconvenient to transport.
Disclose a kind of fluoropolymer or fluorine-containing low molecular compound in US Patent No. 2007028395, process yarn fabric, after making to process, the fabric of gained has good hydro-oleophobicity.Application number 201210058857.X (publication date is 2012.07.25) discloses a kind of two thin polymeric film and preparation method thereof, be made up of POSS base fluorinated block copolymer, with polymethyl monomethacryloxypropyl POSS be the first block, polyacrylic acid hexafluoro butyl ester is the second block.Methacryloxypropyl POSS monomer solution is prepared with solvent, add chain-transfer agent and initiator, be placed in the freezing degassed and sealed reaction after being filled with argon gas of container, liquid nitrogen freezing stopped reaction, with precipitation agent precipitation after solubilizing agent dilution, drying obtains polymethyl monomethacryloxypropyl POSS; Add vinylformic acid hexafluoro butyl ester, initiator and solvent again, the degassed and sealed reaction after being filled with argon gas of freeze thawing, polymerization, liquid nitrogen freezing stopped reaction; Precipitate with the 2nd precipitation agent after adding solvent cut, dry; Be dissolved in again in solvent, be added on substrate, be placed in solvent atmosphere curtain coating and become two thin polymeric film.
Although the two thin material property of current exploitation is very excellent, in finishing composition, still there is emulsifying agent to exist, affect the two thin performance of material; And emulsifying agent often exists with emulsion form, be unfavorable for storing and transport, and fluorochemical monomer amount is higher, causes cost to increase.
Summary of the invention
Provide hereinafter about brief overview of the present invention, to provide about the basic comprehension in some of the present invention.Should be appreciated that this general introduction is not summarize about exhaustive of the present invention.It is not that intention determines key of the present invention or integral part, and nor is it intended to limit the scope of the present invention.Its object is only provide some concept in simplified form, in this, as the preorder in greater detail discussed after a while.
For overcoming the above problems, the invention provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprising the following steps:
1) in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed, 1.5-13.5 part fluorochemical monomer, 2-8 part methyl methacrylate, 1-4 part soft monomer, 2-7 part dimethylaminoethyl methacrylate, 0.1-4 part cross-linking monomer, 0.1-4 part butyl acrylate, 0.1-0.6 part Diisopropyl azodicarboxylate, 10-40 part DMF is added by mass parts;
2) after logical nitrogen deoxidation, heated and stirred, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 1-8h;
3) in there-necked flask, slowly drip 20-45 part Potassium Persulphate saturated aqueous solution by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 1.5-3h, making monomer complete reaction;
4) be cooled to room temperature, discharging, resulting polymers be dissolved in 90-270 part alcoholic solvent, namely can obtain fluorine-containing two thin fabric finishing agent.
Described step 1) in fluorochemical monomer be one or more in perfluor alkyl ethyl acrylate, 2-(perfluor is base) ethylmethyl acrylate, 2-(perfluoro butyl) ethylmethyl acrylate, in 2-(perfluoro capryl) ethylmethyl acrylate, 3-(perfluor-5-methyl base)-2-hydroxy propyl methacrylate.
Described step 1) in soft monomer be one or more in octadecyl acrylate and Process Conditions of Cetane Acrylate.
Described step 1) in cross-linking monomer be one or more in 2-Hydroxy ethyl acrylate, N-hydroxy-succinamide-diazomethane.
Described step 2) Heating temperature is 65-85 DEG C.
Described step 2) stirring velocity is 450-800r/min.
Described step 4) in alcoholic solvent be one or more in methyl alcohol, ethanol, propyl alcohol.
The present invention has following beneficial effect, and fluorine-containing two thin fabric finishing agent prepared by the inventive method is not containing emulsifying agent, and fluorochemical monomer amount is few, and product exists in solid form, is convenient to store and transport, and hydrophobic all better with oleophobic performance.
Embodiment
The following describes embodiments of the invention.The element described in one embodiment of the invention and feature can combine with the element shown in one or more embodiment and feature.It should be noted that for purposes of clarity, in explanation, eliminate expression and the description of unrelated to the invention, parts known to persons of ordinary skill in the art and process.
Embodiment 1
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
1.5 parts of 2-(perfluor is base) ethylmethyl acrylate, 1 part of octadecyl acrylate are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed, 2 parts of methyl methacrylates, 2 parts of dimethylaminoethyl methacrylates, 0.1 part of 2-Hydroxy ethyl acrylate, 0.1 part of butyl acrylate, 0.1 part of Diisopropyl azodicarboxylate, 10 parts of DMFs.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 65 DEG C, and stirring velocity is 450r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 1h.Slowly in there-necked flask, drip 20 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 1.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 90 parts of alcohol solvents, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 2
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
Add in 6 parts of 2-(perfluoro butyl) ethylmethyl acrylate in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed, 2.5 parts of Process Conditions of Cetane Acrylate, 6 parts of methyl methacrylates, 5 parts of dimethylaminoethyl methacrylates, 2 parts of N-hydroxy-succinamide-diazomethanes, 2 parts of butyl acrylates, 0.3 part of Diisopropyl azodicarboxylate, 30 parts of DMFs.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 75 DEG C, and stirring velocity is 600r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 35 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 180 parts of methanol solvates, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 3
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
13.5 parts of 3-(perfluor-5-methyl base)-2-hydroxy propyl methacrylate, 4 parts of octadecyl acrylates are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed, 8 parts of methyl methacrylates, 5 parts of dimethylaminoethyl methacrylates, 4 parts of 2-Hydroxy ethyl acrylates, 4 parts of butyl acrylates, 0.5 part of Diisopropyl azodicarboxylate, 40 parts of DMFs.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 85 DEG C, and stirring velocity is 800r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 8h.Slowly in there-necked flask, drip 45 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 3h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 270 parts of propanol solvent, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 4
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
11 parts of 2-(perfluoro capryl) ethylmethyl acrylate, 3 parts of methyl methacrylates, 1 part of octadecyl acrylate, 2 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 2 parts of butyl acrylates, 0.3 part of Diisopropyl azodicarboxylate, 18 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 77 DEG C, and stirring velocity is 500r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 3h.Slowly in there-necked flask, drip 20 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 170 parts of dehydrated alcohols, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 5
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
10 parts of 2-(perfluor is base) ethylmethyl acrylate, 6 parts of methyl methacrylates, 4 parts of octadecyl acrylates, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.2 part of Diisopropyl azodicarboxylate, 30 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 65 DEG C, and stirring velocity is 700r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 5h.Slowly in there-necked flask, drip 45 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 180 parts of ethanol, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 6
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
2 parts of 2-(perfluor is base) ethylmethyl acrylate, 7 parts of methyl methacrylates, 3 parts of octadecyl acrylates, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.2 part of Diisopropyl azodicarboxylate, 40 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 65 DEG C, and stirring velocity is 750r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 50 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 160 parts of propyl alcohol, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 7
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
8 parts of 2-(perfluoro butyl) ethylmethyl acrylate, 7 parts of methyl methacrylates, 2 parts of Process Conditions of Cetane Acrylate, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.4 part of Diisopropyl azodicarboxylate, 35 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 70 DEG C, and stirring velocity is 700r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 50 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 160 parts of ethanol, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 8
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
3 parts of perfluor alkyl ethyl acrylates, 4 parts of methyl methacrylates, 2 parts of Process Conditions of Cetane Acrylate, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.1 part of Diisopropyl azodicarboxylate, 40 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 65 DEG C, and stirring velocity is 700r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 35 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 190 parts of ethanol, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 9
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
6 parts of perfluor alkyl ethyl acrylates, 4 parts of methyl methacrylates, 2 parts of octadecyl acrylates, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.1 part of Diisopropyl azodicarboxylate, 50 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 70 DEG C, and stirring velocity is 600r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 35 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 190 parts of ethanol, namely can obtain fluorine-containing two thin fabric finishing agent.
Embodiment 10
The present embodiment provides a kind of preparation method of fluorine-containing two thin fabric finishing agent, comprises the following steps:
4 parts of 2-(perfluoro butyl) ethylmethyl acrylate, 4 parts of methyl methacrylates, 2 parts of Process Conditions of Cetane Acrylate, 7 parts of dimethylaminoethyl methacrylates, 2 parts of 2-Hydroxy ethyl acrylates, 3 parts of butyl acrylates, 0.1 part of Diisopropyl azodicarboxylate, 50 parts of DMFs are added in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed.After logical nitrogen deoxidation, heated and stirred, Heating temperature is 70 DEG C, and stirring velocity is 600r/min, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 4h.Slowly in there-necked flask, drip 35 parts of Potassium Persulphate saturated aqueous solutions by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 2.5h, making monomer complete reaction.Be cooled to room temperature, discharging, resulting polymers be dissolved in 180 parts of ethanol, namely can obtain fluorine-containing two thin fabric finishing agent.
Be to be understood that and can carry out various change when not exceeding the spirit and scope of the present invention limited by appended claim, substituting and conversion.And scope of the present invention is not limited only to the specific embodiment of process, equipment, means, method and step described by specification sheets.One of ordinary skilled in the art will readily appreciate that from disclosure of the present invention, can use perform the function substantially identical with corresponding embodiment described herein or obtain and its substantially identical result, existing and that will be developed in the future process, equipment, means, method or step according to the present invention.Therefore, appended claim is intended to comprise such process, equipment, means, method or step in their scope.
Claims (7)
1. a preparation method for fluorine-containing two thin fabric finishing agent, is characterized in that, comprise the steps:
1) in the there-necked flask that reflux condensing tube, stirrer and thermometer are housed, 1.5-13.5 part fluorochemical monomer, 2-8 part methyl methacrylate, 1-4 part soft monomer, 2-7 part dimethylaminoethyl methacrylate, 0.1-4 part cross-linking monomer, 0.1-4 part butyl acrylate, 0.1-0.6 part Diisopropyl azodicarboxylate, 10-40 part DMF is added by mass parts;
2) after logical nitrogen deoxidation, heated and stirred, obtained fluorine-containing two thin fabric finishing agent superpolymer after reaction 1-8h;
3) in there-necked flask, slowly drip 20-45 part Potassium Persulphate saturated aqueous solution by constant pressure funnel, continue insulation and stirrer changed into stirring rod strong stirring 1.5-3h, making monomer complete reaction;
4) be cooled to room temperature, discharging, resulting polymers be dissolved in 90-270 part alcoholic solvent, namely can obtain fluorine-containing two thin fabric finishing agent.
2. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, it is characterized in that, described step 1) in fluorochemical monomer be one or more in perfluor alkyl ethyl acrylate, 2-(perfluor is base) ethylmethyl acrylate, 2-(perfluoro butyl) ethylmethyl acrylate, in 2-(perfluoro capryl) ethylmethyl acrylate, 3-(perfluor-5-methyl base)-2-hydroxy propyl methacrylate.
3. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, is characterized in that, described step 1) in soft monomer be one or more in octadecyl acrylate and Process Conditions of Cetane Acrylate.
4. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, is characterized in that, described step 1) in cross-linking monomer be one or more in 2-Hydroxy ethyl acrylate, N-hydroxy-succinamide-diazomethane.
5. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, is characterized in that, described step 2) Heating temperature is 65-85 DEG C.
6. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, is characterized in that, described step 2) stirring velocity is 450-800r/min.
7. the preparation method of a kind of fluorine-containing two thin fabric finishing agent according to claim 1, is characterized in that, described step 4) in alcoholic solvent be one or more in methyl alcohol, ethanol, propyl alcohol.
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| CN105369624A (en) * | 2015-12-28 | 2016-03-02 | 苏州迈塔斯芯片科技有限公司 | Fluorine-containing finishing agent for hydrophobic and oleophobic fabric and preparation method of fluorine-containing finishing agent |
| CN108300183A (en) * | 2017-09-05 | 2018-07-20 | 湖州加成金属涂料有限公司 | A kind of wrinkle type powdery paints and preparation method |
| CN112391839A (en) * | 2020-11-18 | 2021-02-23 | 湖南派意特服饰有限公司 | Western-style clothes finishing agent and preparation method thereof |
| CN112391839B (en) * | 2020-11-18 | 2023-01-24 | 湖南派意特服饰有限公司 | Western-style clothes finishing agent and preparation method thereof |
| CN113322680A (en) * | 2021-05-31 | 2021-08-31 | 四川轻化工大学 | Short fluorine chain fabric finishing agent and preparation method and application thereof |
| CN113322680B (en) * | 2021-05-31 | 2022-10-25 | 四川轻化工大学 | Short-fluorine-chain fabric finishing agent and preparation method and application thereof |
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Application publication date: 20160120 |