CN100383187C - Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material - Google Patents
Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material Download PDFInfo
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- CN100383187C CN100383187C CNB2005100444802A CN200510044480A CN100383187C CN 100383187 C CN100383187 C CN 100383187C CN B2005100444802 A CNB2005100444802 A CN B2005100444802A CN 200510044480 A CN200510044480 A CN 200510044480A CN 100383187 C CN100383187 C CN 100383187C
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Abstract
The invention discloses a preparing method of politef free-flow graining material, which comprises the following steps: adding politef particle in the solvent; stirring from low-temperature to high-temperature; distilling solvent to collect through heat exchanger; drying residual material to obtain the product.
Description
Technical field
The present invention relates to the manufacture method of tetrafluoroethylene free-flow granulation material.
Background technology
The polytetrafluoroethylene (PTFE) particle micro mist that suspension polymerization is obtained is crushed to more than 10 microns, below 180 microns, carries out the manufacture method that granulation obtains tetrafluoroethylene granulation material then, once proposes many schemes.For example a kind ofly utilize multiple organic solvent to add under the condition that nonionogenic tenside or anion surfactant exist, in the special stirred vessel that contains taper blade, operation steps according to the rules makes the granular polytetrafluoroethylpowder powder that does not contain filler.
But when adopting aforesaid method to make PTFE granulation material, owing to added mixed organic solvents in reaction, after reaction finished, mixed solvent was difficult for reclaiming and being separated, and can only emit.So both polluted environment, improved cost again, and must drop into substantial contribution and administer pollution.In addition, the PTFE granulation material particle that adopts aforesaid method to make, granularity is inhomogeneous, and granular size differs, and the user causes many inconvenience when using this series products.
Summary of the invention
Technical problem to be solved by this invention provides a kind of solvent that utilizes and carries out granulation, and solvent is the manufacture method of the tetrafluoroethylene free-flow granulation material of the recyclable recycling of organic solvent especially, and the tetrafluoroethylene granulation material grain diameter that makes is even.
The manufacture method of tetrafluoroethylene free-flow granulation material of the present invention, it is characterized in that it being that the ptfe micropowder particle is joined in the solvent, start and stir down cooling earlier, and then heat up, in temperature-rise period the distilled solvent is collected through the interchanger condensation, the leftover materials oven dry obtains tetrafluoroethylene granulation material particle.
The PTFE microactuator suspension powder particles that the present invention selects for use must be that particle diameter is even, and median size is between the 10-180 micron.
Described solvent can be a kind of in methyl alcohol, ethanol, Virahol, zellon, trichloromethane, methylene dichloride, trichloroethane, Skellysolve A and the water or any two kinds, preferred adopt single or mixed organic solvents again or the mixed solvent of water and organic solvent, the consumption of solvent is: 100kg ptfe micropowder particle: 200～800 liters of solvents.When two kinds of solvent composition mixed solvents, the amount between them is any proportioning.
The rotating speed of described stirring is preferably 30～2500rpm.
Described temperature-fall period is for to reduce the temperature to-10 ℃ in 0.5～10 hour.
Described temperature-rise period is for to be raised to 10～160 ℃ with temperature in 0.5～15 hour.
Material can be at 50～300 ℃ of oven dry down, granulation material particulate water content≤0.04%.
Advantage of the present invention:
Adopt and mix or single solvent, solvent especially organic solvent can reclaim, and the recycling that can circulate, thereby effectively reduces cost, and prevents to cause the discharging that contains organic solvent waste water, further reduces environmental pollution.The tetrafluoroethylene granulation material volume density that obtains is big, and particle diameter is even, and particle shape is good, good fluidity.
Embodiment:
Embodiment one:
1, the mixed solvent that 2000-2500 is risen the first alcohol and water joins in the reactor.The ratio of first alcohol and water is any ratio.
2,1000kgPTFE suspension micro mist is joined in the scroll feeder, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 2500rpm, cools the temperature to-10 ℃ again in 5-8 hour.Logical then steam heats up, and in 10～15 hours temperature is raised to 130～160 ℃.In temperature-rise period, the distilled mixed solvent is condensed to room temperature through the condensation of interchanger, be collected in again in the middle of the basin with the form of liquid state, and after filtering through filter, can recycle.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 30 hours under 250-300 ℃ environment.
5, be cooled to the room temperature packing.
Embodiment two:
1,1000-1500 being risen the trichloromethane organic solvent joins in the reactor.
2,400-500kgPTFE suspension micro mist is joined in the scroll feeder, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 1200rpm, cools the temperature to-10 ℃ again in 2-4 hour.Logical then steam heats up, and in 8～10 hours temperature is raised to 120 ℃.In temperature-rise period, the distilled organic solvent is condensed to room temperature through the condensation of interchanger, with the form of liquid state be collected in the middle of the basin again and in reactor remaining liquid trichloromethane filter the back through filter and mix, can recycle.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 20 hours under 150-200 ℃ environment.
5, be cooled to the room temperature packing.
Embodiment three:
1,2000 liters of zellons and alcoholic acid mixed organic solvents are joined in the reactor.Zellon and alcoholic acid ratio are any ratios.
2,700-800kgPTFE suspension micro mist is joined in the scroll feeder, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 2300rpm, cools the temperature to-10 ℃ again in 5-7 hour.Logical then steam heats up, and in 8～10 hours temperature is raised to 120～130 ℃.In temperature-rise period, distilled organic solvent zellon and ethanol are condensed to room temperature through the condensation of interchanger, are collected in again in the middle of the basin with the form of liquid state, filter the back with remaining liquid zellon and ethanol in reactor through filter and mix, can recycle.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 18 hours under 150-200 ℃ environment.
5, be cooled to the room temperature packing.
Embodiment four:
1, the mixed solvent with 800 premium on currency and zellon joins in the reactor.Water is any ratio with the ratio of zellon.
2,300～350kgPTFE suspension micro mist is joined in the scroll feeder, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 2000rpm, cools the temperature to-10 ℃ again in 1～2 hour.Logical then steam heats up, and in 3～4 hours temperature is raised to 70～100 ℃.In temperature-rise period, distilled mixed solvent zellon and water are condensed to room temperature through the condensation of interchanger, are collected in the middle of the basin recycle again with the form of liquid state.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 15 hours under 100～150 ℃ environment.
5, be cooled to the room temperature packing.
Embodiment five:
1, the mixed solvent with 800 premium on currency and Skellysolve A joins in the reactor.Water is any ratio with the ratio of Skellysolve A.
2,150～200kgPTFE suspension micro mist is joined in the scroll feeder, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 500rpm, cools the temperature to-10 ℃ again in 4～5 hours.Logical then steam heats up, and in 6～8 hours temperature is raised to 150～160 ℃.In temperature-rise period, distilled mixed solvent Skellysolve A and water are condensed to room temperature through the condensation of interchanger, are collected in the middle of the basin recycle again with the form of liquid state.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 15 hours under 100～150 ℃ environment.
5, be cooled to the room temperature packing.
Embodiment six:
1,800 premium on currency is joined in the reactor.
2,100kgPTFE suspension micro mist is joined-scroll feeder in, start feeder and stir, material is evenly put in the reactor.
3, the rotating speed with reactor is promoted to 2000rpm, cools the temperature to-10 ℃ again in 6～7 hours.Logical then steam heats up, and in 1～3 hour temperature is raised to 100～110 ℃.In temperature-rise period, the distilled water vapor is condensed to room temperature, recycle through the condensation of interchanger.
4, reaction finishes, and material is contained in the drip pan, is put in the Hotaircirculatingoven and dries 20 hours under 200～300 ℃ environment.
5, be cooled to the room temperature packing.
Test result such as following table:
| Test index | Median size | Tensile strength | Elongation at break | Volume density | Mobile |
| Test number | 200-900 μm | ＞24MPa | ＞250％ | ＞800g/L | ＞1000g/min |
| Operative norm | Laser particle size analyzer | HG/T2902-1997 | HG/T2902-1997 | HG/T2900 | ASTMD1895-69 |
There is about 99.7% solvent to be recovered in the reaction process, can recirculation uses after filtering.
Claims (5)
1. the manufacture method of the tetrafluoroethylene free-flow granulation material of a recyclable solvent, it is characterized in that it being that the ptfe micropowder particle is joined in the solvent, cooling earlier under agitation, and then heat up, in temperature-rise period, the distilled solvent is collected through the interchanger condensation, the leftover materials oven dry obtains tetrafluoroethylene granulation material particle, the consumption of wherein said solvent is: 100kg ptfe micropowder particle: 200～800 liters of solvents, described cooling, temperature-rise period was raised to 10～160 ℃ with temperature then for to cool the temperature to-10 ℃ in 0.5～10 hour in 0.5～15 hour.
2. manufacture method according to claim 1 is characterized in that described solvent is one or both in methyl alcohol, ethanol, Virahol, zellon, trichloromethane, methylene dichloride, trichloroethane, Skellysolve A, the water.
3. manufacture method according to claim 1, the rotating speed that it is characterized in that described stirring is 30～2500rpm.
4. manufacture method according to claim 1 is characterized in that described leftover materials are 50～300 ℃ of oven dry down.
5. manufacture method according to claim 1 is characterized in that described ptfe micropowder particulate median size is 10～180 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100444802A CN100383187C (en) | 2005-08-29 | 2005-08-29 | Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100444802A CN100383187C (en) | 2005-08-29 | 2005-08-29 | Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material |
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| Publication Number | Publication Date |
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| CN1923886A CN1923886A (en) | 2007-03-07 |
| CN100383187C true CN100383187C (en) | 2008-04-23 |
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| CNB2005100444802A Active CN100383187C (en) | 2005-08-29 | 2005-08-29 | Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101942163B (en) * | 2010-09-09 | 2013-03-20 | 宁波昌祺氟塑料制品有限公司 | Stirring method and device for PTEE powder |
| CN105835251B (en) * | 2016-03-30 | 2018-12-07 | 济南赛诺富隆新材料有限公司 | A kind of preparation method of polytetrafluoroethylgranule granule |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0673189A (en) * | 1992-08-28 | 1994-03-15 | Daikin Ind Ltd | Method for granulating polytetrafluoroethylene |
| CN1192760A (en) * | 1995-08-11 | 1998-09-09 | 大金工业株式会社 | Process for producing granular powder of modified polytetrafluoroethylene |
| WO1999012996A1 (en) * | 1997-09-08 | 1999-03-18 | Daikin Industries, Ltd. | Lowly chargeable granular polytetrafluoroethylene powder and process for producing the same |
| CN1097068C (en) * | 1997-03-17 | 2002-12-25 | 大金工业株式会社 | Filler-free granular polytetrafluoroethylene powder and process for producing same |
| WO2005003189A1 (en) * | 2003-06-26 | 2005-01-13 | Advanced Technology Materials, Inc. | Polytetrafluoroethylene treatment |
-
2005
- 2005-08-29 CN CNB2005100444802A patent/CN100383187C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0673189A (en) * | 1992-08-28 | 1994-03-15 | Daikin Ind Ltd | Method for granulating polytetrafluoroethylene |
| CN1192760A (en) * | 1995-08-11 | 1998-09-09 | 大金工业株式会社 | Process for producing granular powder of modified polytetrafluoroethylene |
| CN1097068C (en) * | 1997-03-17 | 2002-12-25 | 大金工业株式会社 | Filler-free granular polytetrafluoroethylene powder and process for producing same |
| WO1999012996A1 (en) * | 1997-09-08 | 1999-03-18 | Daikin Industries, Ltd. | Lowly chargeable granular polytetrafluoroethylene powder and process for producing the same |
| WO2005003189A1 (en) * | 2003-06-26 | 2005-01-13 | Advanced Technology Materials, Inc. | Polytetrafluoroethylene treatment |
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| CN1923886A (en) | 2007-03-07 |
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