CN103351474B - A kind of preparation method of Polytetrafluoroethylproduct product surface treatment agent - Google Patents
A kind of preparation method of Polytetrafluoroethylproduct product surface treatment agent Download PDFInfo
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- CN103351474B CN103351474B CN201310287798.8A CN201310287798A CN103351474B CN 103351474 B CN103351474 B CN 103351474B CN 201310287798 A CN201310287798 A CN 201310287798A CN 103351474 B CN103351474 B CN 103351474B
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Abstract
The invention discloses a kind of preparation method of Polytetrafluoroethylproduct product surface treatment agent, by proportioning, the naphthalene of tetraethyleneglycol dimethyl ether 700 grams and 200 grams is added in the four-hole boiling flask of 1 liter of band stirring, start to stir and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene, then in four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add 35.9 grams of sodium Metal 99.5s by proportioning to react, the temperature controlling solution is 80 DEG C, stirring reaction terminates reaction after 5 hours, cooling, close and stir and close nitrogen, the surface treatment agent prepared is poured into be full of in the vial of nitrogen, sealing, keep in Dark Place, Polytetrafluoroethylproduct product surface treatment agent prepared by the inventive method has safety and environmental protection, the advantage that processing power is large, the polytetrafluoroethylproducts products quality obtained after using surface treatment agent process of the present invention is good, qualification rate is high.
Description
Technical field
The present invention relates to a kind of preparation method of fluororesin surface treatment agent, particularly a kind of preparation method for polytetrafluoroethylproducts products surface-treated surface treatment agent.
Background technology
Fluoro-resin particularly tetrafluoroethylene (PTFE) is a kind of macromolecular material of excellent property, there is good chemical stability, electrical insulating property, low frictional coefficient, resistance to chemical attack and higher physical strength, be widely used in the fields such as chemical industry, machinery, aviation, but polytetrafluoroethylmaterial material wettability is poor, the surface energy of goods is low, be unfavorable for bonding, printing and dyeing, application etc., also poor to biocompatibility, thus limit the scope of its application.Therefore must process its surface.
At present, PTFE surface-treated method has ammonia sodium method, biphenyl sodium method, naphthalene sodium etch method, butyl (tetra) titanate-Peroxycaprylic acid coating process, scorification, Corona discharge Treatment method, PTFE surface metal sputtering method, radiation graft process, plasma method etc. in hydrogen or dry ammonia, wherein especially the most simple and practical with naphthalene sodium etch method.Adopt fluororesin surface treatment agent sodium naphthalin treatment solution process polytetrafluoroethylproducts products, treatment solution can destroy C-F key, slough the part fluorine atom on PTFE surface, carburization zone and some polar group is so just left on surface, improve the surfactivity of polytetrafluoroethylproducts products, reduce contact angle, improve surface energy, thus significantly improve can cementability and wetting property.Naphthalene sodium treatment solution is the main material in treatment process, and during preparation, the selection and feed ratio etc. of temperature of reaction, reaction times, solvent all can have an impact to the quality of naphthalene sodium treatment solution, thus has a strong impact on the surface treatment quality of polytetrafluoroethylproducts products.
The preparation of naphthalene sodium treatment solution and treatment process are reported more.
As Tao Xianping in " development of tetrafluoroethylene Local treatment liquid " (" Nantong Vocational College's journal ", volume the 4th phase in December calendar year 2001 the 15th), temperature during formulation of naphthalene-sodium treatment solution, reaction times, naphthalene sodium ratio, solvent are selected and process time PTFE the factor such as temperature be studied.
And for example Chinese patent 200710067500.7 etc. disclose the renovation process of the preparation of naphthalene sodium treatment solution, treatment unit and technique and naphthalene sodium treatment solution.
For another example Chinese patent 200710068976.2 discloses the preparation of naphthalene sodium treatment solution and treatment process.During formulation of naphthalene-sodium treatment solution, temperature of reaction general control is at 0 ~ 30 DEG C, and the reaction times dissolves completely for making sodium Metal 99.5, and solvent selects tetrahydrofuran (THF) usually.The flow process of process PTFE goods is generally first cleans PTFE goods acetone, dries, then with naphthalene sodium treatment solution dipping or coating, then with acetone solvent washing, then washes, dry.Because naphthalene sodium liquid activity is high, is easily hydrolyzed, is oxidized, so in the preparation of naphthalene sodium liquid, use procedure, usually pass into nitrogen protection.
Above the deficiencies in the prior art part is: naphthalene sodium treatment solution solvent for use is volatile, toxicity large, it is heavy to pollute, and preparation execute-in-place environment is poor, is more and more subject to the restriction that environmental requirement improves; Treatment solution corrosive power is weak, and the quality of item after process is poor, there is piebald, corrodes the bad phenomenon such as deep mixed, limits the effect of product.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned prior art present situation, provides the preparation method of the Polytetrafluoroethylproduct product surface treatment agent that the quality of item after a kind of safety and environmental protection, process is good.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of Polytetrafluoroethylproduct product surface treatment agent, comprises the following steps:
(1) add in the four-hole boiling flask of 1 liter of band stirring by the naphthalene of proportioning by tetraethyleneglycol dimethyl ether 700 grams and 200 grams, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene;
(2) in four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, in the obtained solution of step (1), add 35.9 grams of sodium Metal 99.5s by proportioning to react, the temperature controlling solution is 80 DEG C, stirring reaction terminates reaction after 5 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Compared with prior art, the present invention has the following advantages:
1, safety and environmental protection, adopts low toxicity, volatility low, easy recovered solvent preparation Polytetrafluoroethylproduct product surface treatment agent, greatly improves the labor condition of working space, solve the problem of safety in production;
2, the Polytetrafluoroethylproduct product surface treatment agent good fluidity of preparation, processing power is large, significantly reduces the piebald of the rear goods of process, corrodes the bad phenomenon such as deep mixed, improve quality product, reduce further supplies consumption and " three wastes " discharge.
Embodiment
By the following examples more specific description is carried out to the present invention, but the present invention is not limited to described embodiment.
Embodiment 1
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 55.7 grams
Sodium Metal 99.5 10 grams
Glycol dimethyl ether 800 grams
Preparation method is as follows:
By proportioning by glycol dimethyl ether, naphthalene, add in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling reaction solution is 30 DEG C, stirring reaction 3 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 2
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 200 grams
Sodium Metal 99.5 35.9 grams
Tetraethyleneglycol dimethyl ether 700 grams
Preparation method is as follows:
By proportioning, tetraethyleneglycol dimethyl ether, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 80 DEG C, stirring reaction terminates reaction after 5 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 3
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 100 grams
Sodium Metal 99.5 17.8 grams
Diethylene glycol dimethyl ether 700 grams
Preparation method is as follows:
By proportioning, diethylene glycol dimethyl ether, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 80 DEG C, stirring reaction terminates reaction after 10 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 4
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 80 grams
Sodium Metal 99.5 14.4 grams
Diethylene glycol diethyl ether 700 grams
Preparation method is as follows:
By proportioning, diethylene glycol diethyl ether, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 50 DEG C, stirring reaction terminates reaction after 5 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 5
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 279 grams
Sodium Metal 99.5 50 grams
Isosorbide-5-Nitrae-dioxane 600 grams
Preparation method is as follows:
By proportioning, Isosorbide-5-Nitrae-dioxane, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 110 DEG C, stirring reaction terminates reaction after 12 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 6
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 279 grams
Sodium Metal 99.5 11 grams
Diethylene Glycol list ethyl isobutyl ether 600 grams
Preparation method is as follows:
By proportioning, Diethylene Glycol list ethyl isobutyl ether, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 120 DEG C, stirring reaction terminates reaction after 11 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Embodiment 7
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 56 grams
Sodium Metal 99.5 50 grams
Ethylene glycol fourth methyl ether 800 grams
Preparation method is as follows:
By proportioning, ethylene glycol fourth methyl ether, naphthalene are added in the four-hole boiling flask of 1 liter of band stirring, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene; In four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, add required sodium Metal 99.5 by proportioning to react, the temperature controlling solution is 105 DEG C, stirring reaction terminates reaction after 15 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
Comparative example
A kind of Polytetrafluoroethylproduct product surface treatment agent, it is composed as follows:
Naphthalene 500 grams
Sodium Metal 99.5 95 grams
Tetrahydrofuran (THF) 1000 grams
Preparation method is as follows:
By proportioning, tetrahydrofuran (THF) is added in 3000ml there-necked flask, put into ice bath and stir cooling; Temperature controls at 20 DEG C; Slowly add after required naphthalene stirs at room temperature and atmospheric pressure, fresh sodium sheet is divided three times and adds in flask, every minor tick 20 minutes, and constantly stir, make it whole dissolving, be i.e. obtained surface treatment agent.
Embodiment 8 ~ 15
The performance test of the Polytetrafluoroethylproduct product surface treatment agent process polytetrafluoroethylproducts products that embodiment 1 ~ 7 and comparative example obtain.Wherein product surface piebald appearance method detects, and product surface contact angle water droplet method is tested.
The processing step of process polytetrafluoroethylproducts products is: first good to turning polytetrafluoroethylproducts products, with acetone or alcohol washes, and removing surface and oil contaminant and foul; Clean polytetrafluoroethylproducts products is immersed dipping in the surface treatment agent filling and prepared to take out after 2 minutes; First with normal-temperature water cleaning, then put into 90 DEG C of hot water and clean, residue such as removing NaH and naphthalene etc., takes out polytetrafluoroethylproducts products acetone and water is clean cleansing article, dries, pack.The results are shown in Table 1
The result of the surface treatment agent process polytetrafluoroethylproducts products that table 1 embodiment 1 ~ 7 and comparative example obtain
Claims (1)
1. a preparation method for Polytetrafluoroethylproduct product surface treatment agent, is characterized in that comprising the following steps:
(1) add in the four-hole boiling flask of 1 liter of band stirring by the naphthalene of proportioning by tetraethyleneglycol dimethyl ether 700 grams and 200 grams, start stirring and naphthalene is stirred to whole dissolving, obtain the solution containing naphthalene;
(2) in four-hole boiling flask, dry nitrogen is passed into 500mL/min flow, in the obtained solution of step (1), add 35.9 grams of sodium Metal 99.5s by proportioning to react, the temperature controlling solution is 80 DEG C, stirring reaction terminates reaction after 5 hours, cooling, closes and stirs and close nitrogen, the surface treatment agent prepared is poured into and is full of in the vial of nitrogen, sealing, keeps in Dark Place.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432901A (en) * | 2011-08-05 | 2012-05-02 | 巨化集团公司 | Method for treating surface of polytetrafluoroethylene product with sodium naphthalene solution |
| CN102558592A (en) * | 2011-12-02 | 2012-07-11 | 常熟市何市教育橡塑厂 | Preparation method for sodium-naphthaline treatment fluid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432901A (en) * | 2011-08-05 | 2012-05-02 | 巨化集团公司 | Method for treating surface of polytetrafluoroethylene product with sodium naphthalene solution |
| CN102558592A (en) * | 2011-12-02 | 2012-07-11 | 常熟市何市教育橡塑厂 | Preparation method for sodium-naphthaline treatment fluid |
Non-Patent Citations (2)
| Title |
|---|
| 多层微带线路板制造技术研究;杨维生;《电子工艺技术》;20050930;第26卷(第5期);第267-272页 * |
| 聚四氟乙烯局部处理液的研制;陶贤平;《南通职业大学学报》;20011231;第15卷(第4期);第41-43页 * |
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Inventor after: Xu Hong Inventor after: Jing Yabin Inventor after: Yan Huahong Inventor after: Tong Wenliang Inventor after: Wu Yi Inventor before: Xu Xiazhong Inventor before: Xu Hong Inventor before: Jing Yabin Inventor before: Yan Huahong Inventor before: Tong Wenliang Inventor before: Wu Yi |
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Effective date of registration: 20180920 Address after: 324022 No. seven Donggang Road, Kecheng Industrial Park, Quzhou, Zhejiang, 118 Co-patentee after: Juhua Group Co., Ltd. Patentee after: Zhejiang Green New Materials Co., Ltd. Address before: 324022 No. seven Donggang Road, Kecheng Industrial Park, Quzhou, Zhejiang, 118 Co-patentee before: Technology Center of Juhua Group Patentee before: Zhejiang Green New Materials Co., Ltd. |
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