CN101307166A - Grained polytetrafluorethylene for filling and method for preparing same - Google Patents
Grained polytetrafluorethylene for filling and method for preparing same Download PDFInfo
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- CN101307166A CN101307166A CNA2007100178748A CN200710017874A CN101307166A CN 101307166 A CN101307166 A CN 101307166A CN A2007100178748 A CNA2007100178748 A CN A2007100178748A CN 200710017874 A CN200710017874 A CN 200710017874A CN 101307166 A CN101307166 A CN 101307166A
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Abstract
The invention relates to granular filled polytetrafluoroethylene and a method for preparing the same. The granular filled polytetrafluoroethylene is characterized by comprising the following compositions: polytetrafluoroethylene, barium sulfate, distilled water, organic liquid and surface active agent. The preparation method comprises the following steps that: firstly, the barium sulfate and polytetrafluoroethylene micro powder are mechanically mixed through the conventional dry method to obtain filled polytetrafluoroethylene micro powder; secondly, the filled polytetrafluoroethylene micro powder, the surface active agent and the distilled water are added into a reaction kettle in turn, stirred for 3 to 5 minutes and then added with the organic liquid, and the process is finished between 5 and 30 minutes; the mixture is continuously stirred for 0 to 30 minutes, and the stirring speed is controlled within the range between 800 and 1200 turns per minute during the whole granulation process; thirdly, the mixture is washed by water for a plurality of times and dried, and then the granular filled polytetrafluoroethylene is obtained. The granular filled polytetrafluoroethylene provided by the invention has a regular shape, small mean diameter, narrow grain diameter distribution, superior powder fluidity, high apparent density and easiness in forming. The preparation method is simple and easy and has stable technique.
Description
Technical field
The present invention relates to a kind of grained polytetrafluorethylefor for filling and preparation method thereof, belong to processing of high molecular material and Application Areas.
Background technology
That tetrafluoroethylene has is heat-resisting, cold-resistant, chemical proofing and good weathering resistance, and have characteristics such as special electrical property, surface property, non-viscosity, self lubricity and low-friction coefficient, be widely used in many fields such as national defence, military project, space flight and aviation, automobile, petrochemical complex.But because the PTFE powder flowbility is poor, apparent density is low, is not suitable for the automatic extruding process.And because the requirement and moulding specific (or special) product requirements of the production automation need the PTFE resin to have good powder flowbility and high apparent density.
External more in the research in this field, technology maturation, the production of grained polytetrafluorethylefor for filling is many to be finished by PTFE production of resins company, as the G300 series of Japan AGC company and M-390 series, 8 series of du pont company and 1600 series of 3M company etc. of big King Company.And, according to usable conditions such as products appearance, article shape and High-Speed Automatic mold pressings, carried out deep classification.The grained polytetrafluorethylefor for filling of its different trades mark all has comparatively clear and definite applicable situation.Though domestic also have some companies to produce and sell granular tetrafluoroethylene product, its product is single, and there are very big gap in performance, quality stability etc. with external like product.
In addition, United States Patent (USP) 4241137 and 6203733B1 have announced the liquid-liquid granulation process that does not need tensio-active agent, but the method that above-mentioned patent is announced can not get the granular tetrafluoroethylene of the little and narrow diameter distribution of particle diameter.In United States Patent (USP) 6451903B1,6458457B1,6350801B1 and 6197862B1, and all announced in the Chinese patent 01117153.7,96197046.4,96197856.2,98803199.X, 98803200.7 and 98804388.2 comparatively similarly, the method for preparing grained polytetrafluorethylefor for filling under water-fast organic liquid and aniorfic surfactant or nonionic surface active agent acting in conjunction.But the method complex process that provides in the above-mentioned patent needs the segmentation speed change to stir, even needs heating.United States Patent (USP) 6281281B1 and 6440559B1 and Chinese patent 96198202.0,98803188.4 and 98804391.2 have been announced the dry granulation process method under aniorfic surfactant or nonionic surface active agent effect, but because aforesaid method needs special-purpose swivel base formula high-speed mixing equipment, technology cost height.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of grained polytetrafluorethylefor for filling and preparation method thereof, and stirring velocity does not need sectional-regulatedly in the granulating process, remains on certain limit and gets final product, and does not also need heating and specialized apparatus.Prepared grained polytetrafluorethylefor for filling regular shape, median size are little, narrow diameter distribution, powder flowbility excellence.
Technical scheme
Technical characterictic of the present invention is that the component prescription is as follows: tetrafluoroethylene: 70 mass ratioes, barium sulfate 325 orders: 30 mass ratioes, distilled water: 200～600 mass ratioes, organic liquid: 30～100 mass ratioes, tensio-active agent: 0.01～1.00 mass ratio.
Described organic liquid is: alcohol, ether, ketone, aliphatic hydrocarbon, aromatic hydrocarbons and halohydrocarbon.
Described halohydrocarbon is chloro and hydrofluoric ether.As, methylene dichloride, zellon, trieline, chloroform, chlorobenzene, Refrigerant R 113, trichloromethane, difluoro tetrachloroethane, 1,1,1-trichloroethane, 1,1-two chloro-2,2,3,3,3-pentafluoropropane, 1,3-two chloro-1,1,2,2,3-pentafluoropropane, 1,1-two chloro-1-fluoroethanes and 1,1-two chloro-2,2,2-Halothane etc.
Described tensio-active agent is: nonionic surface active agent and aniorfic surfactant.
Described nonionic surface active agent is: polyoxy ethamine, alkylamine, Voranol EP 2001, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, sorbitan fatty acid ester, polyxyethylated by, polyalkylene glycol and polyoxyethylene-polyoxypropylene block polyether.
Described aniorfic surfactant is: higher fatty acid and its esters, alkyl-sulphate, alkylsulfonate, alkylaryl sulphonate and alkyl phosphate.Especially, the senior alkyl alcohol sulfate, as sodium lauryl sulphate, fluorine-containing sulfuric acid type or carboxylic acid type anion surfactant (having fluoroalkyl or freon base).
A kind of method for preparing grained polytetrafluorethylefor for filling is characterized in that preparation process is as follows:
Step 1, at first get the filled polytetrafluoroethylene micro mist by conventional dry method mechanically mixing barium sulfate and ptfe micropowder;
Step 2, the ptfe micropowder that then above-mentioned filling is obtained, tensio-active agent and distilled water add in the reactor successively, stir and drip organic liquid after 3～5 minutes, added in 5～30 minutes, continue to stir 0～30 minute, stirring velocity is controlled in 800～1200 rev/mins of scopes in whole granulating process;
Step 3, last washed several times with water, drying promptly gets grained polytetrafluorethylefor for filling.
Guarantee that organic liquid and the surface tension of water mixture in the time of 25 degrees centigrade should not be higher than every centimetre of 35 dyne.Under aniorfic surfactant or nonionic surface active agent effect, can form liquid-liquid interface and be scattered in the water with small droplets with water.
Beneficial effect
Its main component of grained polytetrafluorethylefor for filling that the present invention proposes is 30% barium sulfate (mass percent, a down together) filled polytetrafluoroethylene.Wet method granulation is adopted in its preparation, and the filled polytetrafluoroethylene micro mist that is pre-mixed is wetting with organic liquid, forms liquid-liquid interface through different alr mode cohesion granulating with water under aniorfic surfactant or nonionic surface active agent effect.Advantage of the present invention is:
(1) simple, the process stabilizing of novel method of preparation grained polytetrafluorethylefor for filling proposed by the invention.
(2) little, the narrow diameter distribution of grained polytetrafluorethylefor for filling regular shape provided by the present invention, median size, powder flowbility excellence, apparent density height and easy-formation.
(3) the pressing tensile strength and the elongation at break excellence of grained polytetrafluorethylefor for filling preparation provided by the present invention.
Description of drawings
Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5 are respectively the polarizing microscope photo by example 1, example 2, example 3, example 4 and example 5 gained grained polytetrafluorethylefor for filling, and magnification is 40 times.
Embodiment
Now the present invention is further described:
Embodiment 1: add 20 grams, 30% barium sulfate filled polytetrafluoroethylene micro mist, 1～2 milliliter of 5% Perfluorocaprylic Acid ammonia soln and 60 gram distilled water in the reactor successively, stir and drip 15.6 gram organic liquid methylene dichloride after 3～5 minutes, added in 5～10 minutes, continue to stir 3～5 minutes, filter, washed several times with water, drying promptly gets the grained polytetrafluorethylefor for filling (see figure 1).
Embodiment 2: add 20 grams, 30% barium sulfate filled polytetrafluoroethylene micro mist, 5～10 milliliter of 1% sodium dodecyl benzene sulfonate aqueous solution and 60 gram distilled water in the reactor successively, stir and drip 15.6 gram organic liquid methylene dichloride after 3～5 minutes, added in 5～10 minutes, continue to stir 0～20 minute, filter, washed several times with water, drying promptly gets the grained polytetrafluorethylefor for filling (see figure 2).
Embodiment 3: add 20 grams, 30% barium sulfate filled polytetrafluoroethylene micro mist, 1～2 milliliter of 1% perfluorinated nonene oxygen base benzene sulfonic acid sodium salt (FBS) aqueous solution and 60 gram distilled water in the reactor successively, stir and drip 15.6 gram organic liquid methylene dichloride after 3～5 minutes, added in 5～15 minutes, continue to stir 0～20 minute, filter, washed several times with water, drying promptly gets the grained polytetrafluorethylefor for filling (see figure 3).
Embodiment 4: add 20 grams, 30% barium sulfate filled polytetrafluoroethylene micro mist, 1 milliliter of 5% polyoxy ethamine (OA-12) aqueous solution and 60 gram distilled water in the reactor successively, stir and drip 15.6 gram organic liquid methylene dichloride after 3～5 minutes, added in 5～15 minutes, continue to stir 3～10 minutes, filter, washed several times with water, drying promptly gets the grained polytetrafluorethylefor for filling (see figure 4).
Embodiment 5: add 20 grams, 30% barium sulfate filled polytetrafluoroethylene micro mist, 1 milliliter of 5% polyoxyethylene-polyoxypropylene block polyether polyethers (L42) aqueous solution and 60 gram distilled water in the reactor successively, stir and drip 15.6 gram organic liquid methylene dichloride after 3～5 minutes, added in 5～20 minutes, continue to stir 0～5 minute, filter, washed several times with water, drying promptly gets the grained polytetrafluorethylefor for filling (see figure 5).
Table 1 is the partial properties data by example 1, example 2, example 3, example 4 and example 5 gained grained polytetrafluorethylefor for filling.
Table 1
Annotate: tensile strength and elongation at break are the performance datas of 30% barium sulfate filled polytetrafluoroethylene pellet pressing.
Claims (8)
1. grained polytetrafluorethylefor for filling, it is characterized in that the component prescription is as follows: tetrafluoroethylene: 70 mass ratioes, barium sulfate 325 orders: 30 mass ratioes, distilled water: 200～600 mass ratioes, organic liquid: 30～100 mass ratioes, tensio-active agent: 0.01～1.00 mass ratio.
2. grained polytetrafluorethylefor for filling according to claim 1 is characterized in that: described organic liquid is: alcohol, ether, ketone, aliphatic hydrocarbon, aromatic hydrocarbons and halohydrocarbon.
3. grained polytetrafluorethylefor for filling according to claim 2 is characterized in that: described halohydrocarbon is chloro and hydrofluoric ether.
4. grained polytetrafluorethylefor for filling according to claim 1 is characterized in that: described tensio-active agent is: nonionic surface active agent and aniorfic surfactant.
5. grained polytetrafluorethylefor for filling according to claim 4 is characterized in that: described nonionic surface active agent is: polyoxy ethamine, alkylamine, Voranol EP 2001, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, sorbitan fatty acid ester, polyxyethylated by, polyalkylene glycol and polyoxyethylene-polyoxypropylene block polyether.
6. grained polytetrafluorethylefor for filling according to claim 4 is characterized in that: described aniorfic surfactant is: higher fatty acid and its esters, alkyl-sulphate, alkylsulfonate, alkylaryl sulphonate and alkyl phosphate.
7. method for preparing the described grained polytetrafluorethylefor for filling of claim 1～6 is characterized in that preparation process is as follows:
Step 1, at first get the filled polytetrafluoroethylene micro mist by conventional dry method mechanically mixing barium sulfate and ptfe micropowder;
Step 2, the ptfe micropowder that then above-mentioned filling is obtained, tensio-active agent and distilled water add in the reactor successively, stir and drip organic liquid after 3～5 minutes, added in 5～30 minutes, continue to stir 0～30 minute, stirring velocity is controlled in 800～1200 rev/mins of scopes in whole granulating process;
Step 3, last washed several times with water, drying promptly gets grained polytetrafluorethylefor for filling.
8. grained polytetrafluorethylefor for filling according to claim 7 is characterized in that: guarantee that organic liquid and the surface tension of water mixture in the time of 25 degrees centigrade should not be higher than every centimetre of 35 dyne.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100178748A CN101307166A (en) | 2007-05-17 | 2007-05-17 | Grained polytetrafluorethylene for filling and method for preparing same |
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| CNA2007100178748A CN101307166A (en) | 2007-05-17 | 2007-05-17 | Grained polytetrafluorethylene for filling and method for preparing same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627819A (en) * | 2011-07-12 | 2012-08-08 | 天津市天塑科技集团有限公司技术中心 | Barium sulfate filled modified PTFE resinoid |
| CN108822313A (en) * | 2018-07-18 | 2018-11-16 | 合肥安力电力工程有限公司 | A kind of preparation method of polytetrafluoroethylene (PTFE) pellet |
-
2007
- 2007-05-17 CN CNA2007100178748A patent/CN101307166A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627819A (en) * | 2011-07-12 | 2012-08-08 | 天津市天塑科技集团有限公司技术中心 | Barium sulfate filled modified PTFE resinoid |
| CN108822313A (en) * | 2018-07-18 | 2018-11-16 | 合肥安力电力工程有限公司 | A kind of preparation method of polytetrafluoroethylene (PTFE) pellet |
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Open date: 20081119 |