CN105835251A - Preparation method of polytetrafluoroethylene particles - Google Patents

Preparation method of polytetrafluoroethylene particles Download PDF

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Publication number
CN105835251A
CN105835251A CN201610189559.2A CN201610189559A CN105835251A CN 105835251 A CN105835251 A CN 105835251A CN 201610189559 A CN201610189559 A CN 201610189559A CN 105835251 A CN105835251 A CN 105835251A
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Prior art keywords
granule
preparation
hours
comminutor
polytetrafluoroethylgranule
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CN201610189559.2A
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Chinese (zh)
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CN105835251B (en
Inventor
谭江玲
窦圣堂
王化文
杨丽
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Jinan Sinoflon New Material Co Ltd
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Jinan Sinoflon New Material Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/02Making granules by dividing preformed material
    • B29B9/06Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00Conditioning or physical treatment of the material to be shaped
    • B29B13/06Conditioning or physical treatment of the material to be shaped by drying
    • B29B13/065Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/16Auxiliary treatment of granules

Abstract

The invention relates to a preparation method of polytetrafluoroethylene particles. The preparation method comprises adding a mixed solvent into polytetrafluoroethylene fine powder, carrying out standing and stirring, putting the mixture into a pelletizer, preparing primary particles, carrying out compaction through a compaction machine and carrying out drying to obtain polytetrafluoroethylene particles. The polytetrafluoroethylene particles have the average grain diameter of 300-700 microns and particle bulk density of 850-900g/l. The preparation method solves micro-powder agglomeration, is free of temperature control in production so that energy consumption is reduced, and consumes less organic solvent or water. The polytetrafluoroethylene particles are uniform and have regular shapes, narrow particle size distribution and good fluidity.

Description

A kind of preparation method of polytetrafluoroethylgranule granule
Technical field
The present invention relates to a kind of prilling, particularly relate to the preparation method of a kind of polytetrafluoroethylgranule granule.
Background technology
Politef is the engineering plastics of a kind of function admirable, is widely used in every profession and trade.Owing to its melt temperature is high, melt viscosity is big, therefore be not suitable for the forming method that common plastics melt extrudes, melts injection.
It is low that suspension method obtains polytetrafluorethylepowder powder bulk density, poor fluidity, and easily conglomeration, is only used for common artificial mold pressing, and the little product high for automatic extruding and fineness or thin wall parts then cannot meet.By polytetrafluorethylepowder powder is carried out pelletize, the bulk density of PTFE can be improved, improve its mobility, meet the process requirements of large-duty automatic extruding and some fine goods.
The pelletize in a wet process of existing granulating technique is main.Chinese patent 201010217168.X discloses the manufacture method of a kind of granular polytetrafluoroethylpowder powder, and finished product ptfe micropowder granule can be reunited in transport and storing process, and the greatest problem run in granulation process is exactly the reunion of micropowder.In the method, the politef fine grained used by pelletize is necessary " fresh ", namely must have the disintegrating apparatus of politef.Temperature to be controlled in mixed process, to heat up in granulation process, and insulation, these all can increase energy consumption., there is energy waste and washes emission problem in the removal step of organic liquid.Ptfe micropowder or fine grained stir granulating the most at random, and become granule is it is difficult to ensure that uniform particle sizes.
Chinese patent 200510044480.2 discloses the manufacture method of the politef free-flowing granulation material of solvent-recoverable.The method defect is: relatively low low temperature to prevent ptfe micropowder from reuniting, rising temperature reclamation solvent again, and after first low temperature, high temperature increases energy consumption;And solvent load is relatively big, the most volatile totally, carry organic solvent secretly and can reduce properties of product.
Summary of the invention
For solving the problems referred to above, the present invention provides the preparation method of a kind of polytetrafluoroethylgranule granule, solves micropowder agglomeration traits, production process need not control temperature, saves solvent load, and prepared polytetrafluoroethylgranule granule is uniform, regular shape, size is controlled, good fluidity.
The present invention is achieved by the following technical solutions:
The preparation method of a kind of polytetrafluoroethylgranule granule, it is characterised in that comprise the following steps:
(1) add the mixed solvent of organic solvent and water to fine polytetrafluoroethylpowder powder, stir 15~30 minutes after placing 5~10 hours, once break up;
(2) material broken up in step (1) puts into comminutor, and secondary is broken up, and extrudes from sieve plate, makes primary granule;
(3) during primary granule puts into pre-pressing machine, rolling 5~15 minutes, granule is closely knit;
(4) dry 18~25 hours at 120~280 DEG C during granule inserts drying tray, obtain polytetrafluoroethylgranule granule.
Preferably, the speed of agitator described in step (1) is 20~50rpm;Comminutor rotating speed described in step (2) is 3200~4000rpm;Hole diameter of sieve (perforated) plate in comminutor is 0.5~2mm;Pre-pressing machine chassis rotating speed described in step (3) is 300~600rpm.
It is highly preferred that the speed of agitator described in step (1) is 30rpm;Comminutor rotating speed described in step (2) is 3200~3500rpm;The hole diameter of sieve (perforated) plate of comminutor is 0.8~1.5mm;Pre-pressing machine chassis rotating speed described in step (3) is 400~500rpm.
Preferably, the consumption of the solvent described in step (1) is: 100kg fine polytetrafluoroethylpowder powder: 20~50kg solvents;Solvent is that in ethanol, isopropanol, one or both form mixed solvent with water, and consumption of organic solvent is more than the consumption of water.
Preferably, step (4) described drying is first to be warming up to 120~150 DEG C, constant temperature 10 hours, then is warming up to 250~280 DEG C, constant temperature 10 hours.
Preferably, in step (1), the mean diameter of fine polytetrafluoroethylpowder powder is 5~50 microns.
The preparation method of a kind of polytetrafluoroethylgranule granule of the present invention, is not only suitable for the production of pure polytetrafluoroethylgranule granule material, is also suitable for filling the production of the polytetrafluoroethylgranule granule material of reinforcing material.Reinforcing material is known in the art any commonly employed reinforcing material, such as: the fibrous material such as glass fibre, carbon fiber, the metal powder material such as copper powder, stainless steel powder, the inorganic material in powder form such as coke blacking, graphite and the new organic materials such as polybenzoate, polyimides.The manufacture of the polytetrafluoroethylgranule granule material of reinforcing material, wanted first according to corresponding proportioning batch mixing in high speed mixer before solubilizer.
Polytetrafluoroethylgranule granule prepared by the present invention, mean diameter can be controlled between 300~700 microns, pure polytetrafluoroethylgranule granule material bulk density 850~900g/l, politef pellet containing reinforcing material changes with bulk density and the loading of reinforcing material, powder fluidity 1.5~2.5s/100g, product moisture content 0.01%~0.02%.
Beneficial effects of the present invention:
1. the preparation method of a kind of polytetrafluoroethylgranule granule that the present invention provides, micropowder agglomeration traits has been resolved in process of production, and production process need not control temperature, and energy consumption reduces;Consume organic solvent or water is fewer;The polytetrafluoroethylgranule granule prepared is uniform, regular shape, narrow diameter distribution, good fluidity.
2. the one during the solvent selected by the present invention is ethanol, isopropanol, miscible with water, readily volatilized, and human non-toxic's evil solvent is added in fine polytetrafluoroethylpowder powder.Place a period of time, solvent penetration fine polytetrafluoroethylpowder powder can be made.Stir before politef pelletize, solvent can be made to mix homogeneously with material, the politef material group of mixed solvent is broken up, material secondary in comminutor can be made to be more readily formed uniform granule when breaing up.It is extruded into primary particle by the screen cloth that aperture is consistent, improves rotating speed, make particle diameter more uniform;Again by controlling time rolling densification, on the one hand regular particles can be made spherical in shape, on the other hand granule can be made to reach the bulk density wanted.
The scope of application the most of the present invention is more extensive, both can be applicable to the production of pure polytetrafluoroethylgranule granule material, it is possible to be applied to fill the production of the polytetrafluoroethylgranule granule material of reinforcing material.
Detailed description of the invention
Embodiment 1
(1) fine polytetrafluoroethylpowder powder 100kg(Zhong Hao Chenguang Research Institute of Chemical Industry suspension fine powder CGM16F mean diameter 25 microns is taken) join in the container of cleaning, the mixing liquid of 20kg ethanol and deionized water is sprayed in above-mentioned fine polytetrafluoroethylpowder powder, ethanol quality is 2:1 with the mass ratio of water, after placing 5 hours, it is placed under the agitator of 20rpm stirring 15 minutes, fine polytetrafluoroethylpowder powder is once broken up.
(2) fine polytetrafluoroethylpowder powder of mixed solvent being put into comminutor continuously, rotating speed is 3200rpm, and fine powder secondary is dispersed as little granule, and little granule is extruded from sieve plate, and hole diameter of sieve (perforated) plate is 0.5mm, makes primary granule.
(3) primary granule is with in each 10kg Input Level rotating disk pre-pressing machine, and chassis rotating speed is 300rpm, rotates 5 minutes, primary granule, with the rotation on chassis, rolls, phase mutual friction between material particles in barrel, material particles and material tube inner wall friction, granule is round as a ball, and granule becomes closely knit.
(4) fine and close good granule is inserted in drying tray, put in the baking oven of inner-outer circulation device, be first warming up to 120 DEG C, constant temperature 10 hours, then it is warming up to 250 DEG C, and constant temperature 10 hours, obtain polytetrafluoroethylgranule granule.
Embodiment 2
(1) fine polytetrafluoroethylpowder powder 100kg(Shandong Dongyue Polymer Material Co., Ltd. suspension fine powder DF-16A mean diameter 5 microns is taken), join in the container of cleaning, the mixing liquid of 50kg isopropanol and deionized water is sprayed in above-mentioned fine polytetrafluoroethylpowder powder, isopropanol quality is 3:1 with the mass ratio of water, after placing 10 hours, it is placed under the agitator of 50rpm stirring 30 minutes, fine polytetrafluoroethylpowder powder is once broken up.
(2) fine polytetrafluoroethylpowder powder of mixed solvent being put into comminutor continuously, rotating speed is 3500rpm, and fine powder secondary is dispersed as little granule, and little granule is extruded from sieve plate, and hole diameter of sieve (perforated) plate is 2.0mm, makes primary granule.
(3) primary granule is with in each 10kg Input Level rotating disk pre-pressing machine, and chassis rotating speed is 600rpm, rotates 15 minutes, primary granule, with the rotation on chassis, rolls, phase mutual friction between material particles in barrel, material particles and material tube inner wall friction, granule is round as a ball, and granule becomes closely knit.
(4) fine and close good granule is inserted in drying tray, put in the baking oven of inner-outer circulation device, be first warming up to 150 DEG C, constant temperature 10 hours, then it is warming up to 280 DEG C, and constant temperature 10 hours, obtain polytetrafluoroethylgranule granule.
Embodiment 3
(1) fine polytetrafluoroethylpowder powder 100kg(Zhong Hao Chenguang Research Institute of Chemical Industry suspension fine powder CGM16F mean diameter 22 microns is taken), join in the container of cleaning, the mixing liquid of 40kg isopropanol and deionized water is sprayed in above-mentioned fine polytetrafluoroethylpowder powder, isopropanol quality is 3:2 with the mass ratio of water, after placing 7 hours, it is placed under the agitator of 30rpm stirring 15 minutes, fine polytetrafluoroethylpowder powder is once broken up.
(2) fine polytetrafluoroethylpowder powder of mixed solvent being put into comminutor continuously, rotating speed is 4000rpm, and fine powder secondary is dispersed as little granule, and little granule is extruded from sieve plate, and hole diameter of sieve (perforated) plate is 0.8mm, makes primary granule.
(3) primary granule is with in each 10kg Input Level rotating disk pre-pressing machine, and chassis rotating speed is 500rpm, rotates 8 minutes, primary granule, with the rotation on chassis, rolls, phase mutual friction between material particles in barrel, material particles and material tube inner wall friction, granule is round as a ball, and granule becomes closely knit.
(4) fine and close good granule is inserted in drying tray, put in the baking oven of inner-outer circulation device, be first warming up to 120 DEG C, constant temperature 8 hours, then it is warming up to 280 DEG C, and constant temperature 10 hours, obtain polytetrafluoroethylgranule granule.
Embodiment 4
(1) fine polytetrafluoroethylpowder powder 100kg(Zhong Hao Chenguang Research Institute of Chemical Industry suspension fine powder CGM16F mean diameter 50 microns is taken), join in the container of cleaning, the mixing liquid of 38kg isopropanol and deionized water is sprayed in above-mentioned fine polytetrafluoroethylpowder powder, isopropanol quality is 5:2 with the mass ratio of water, after placing 8 hours, it is placed under the agitator of 30rpm stirring 20 minutes, fine polytetrafluoroethylpowder powder is once broken up.
(2) fine polytetrafluoroethylpowder powder of mixed solvent being put into comminutor continuously, rotating speed is 3300rpm, and fine powder secondary is dispersed as little granule, and little granule is extruded from sieve plate, and hole diameter of sieve (perforated) plate is 1.5mm, makes primary granule.
(3) primary granule is with in each 10kg Input Level rotating disk pre-pressing machine, and chassis rotating speed is 500rpm, rotates 12 minutes, primary granule, with the rotation on chassis, rolls, phase mutual friction between material particles in barrel, material particles and material tube inner wall friction, granule is round as a ball, and granule becomes closely knit.
(4) fine and close good granule is inserted in drying tray, put in the baking oven of inner-outer circulation device, be first warming up to 150 DEG C, constant temperature 8 hours, then it is warming up to 250 DEG C, and constant temperature 10 hours, obtain polytetrafluoroethylgranule granule.
Embodiment 5
(1) fine polytetrafluoroethylpowder powder 50kg(Zhong Hao Chenguang Research Institute of Chemical Industry suspension fine powder CGM16F mean diameter 22 microns is taken), join in the container of cleaning, the mixing liquid of 30kg isopropanol and deionized water is sprayed in above-mentioned fine polytetrafluoroethylpowder powder, isopropanol quality is 3:2 with the mass ratio of water, after placing 9 hours, it is placed under the agitator of 30rpm stirring 30 minutes, fine polytetrafluoroethylpowder powder is once broken up.
(2) fine polytetrafluoroethylpowder powder of mixed solvent being put into comminutor continuously, rotating speed is 3300rpm, and fine powder secondary is dispersed as little granule, and little granule is extruded from sieve plate, and hole diameter of sieve (perforated) plate is 1.2mm, makes primary granule.
(3) primary granule is with in each 10kg Input Level rotating disk pre-pressing machine, and chassis rotating speed is 400rpm, rotates 10 minutes, primary granule, with the rotation on chassis, rolls, phase mutual friction between material particles in barrel, material particles and material tube inner wall friction, granule is round as a ball, and granule becomes closely knit.
(4) fine and close good granule is inserted in drying tray, put in the baking oven of inner-outer circulation device, be first warming up to 150 DEG C, constant temperature 10 hours, then it is warming up to 280 DEG C, and constant temperature 10 hours, obtain polytetrafluoroethylgranule granule.
The polytetrafluoroethylgranule granule parameters made:

Claims (6)

1. the preparation method of a polytetrafluoroethylgranule granule, it is characterised in that comprise the following steps:
(1) add the mixed solvent of organic solvent and water to fine polytetrafluoroethylpowder powder, stir 15~30 minutes after placing 5~10 hours, once break up;
(2) material broken up in step (1) puts into comminutor, and secondary is broken up, and extrudes from sieve plate, makes primary granule;
(3) during primary granule puts into pre-pressing machine, rolling 5~15 minutes, granule is closely knit;
(4) dry 18~25 hours at 120~280 DEG C during granule inserts drying tray, obtain polytetrafluoroethylgranule granule.
The preparation method of a kind of polytetrafluoroethylgranule granule the most as claimed in claim 1, it is characterised in that the speed of agitator described in step (1) is 20~50rpm;Comminutor rotating speed described in step (2) is 3200~4000rpm;Hole diameter of sieve (perforated) plate in comminutor is 0.5~2mm;Pre-pressing machine chassis rotating speed described in step (3) is 300~600rpm.
The preparation method of a kind of polytetrafluoroethylgranule granule the most as claimed in claim 2, it is characterised in that the speed of agitator described in step (1) is 30rpm;Comminutor rotating speed described in step (2) is 3200~3500rpm;The hole diameter of sieve (perforated) plate of comminutor is 0.8~1.5mm;Pre-pressing machine chassis rotating speed described in step (3) is 400~500rpm.
The preparation method of a kind of polytetrafluoroethylgranule granule the most as claimed in claim 1, it is characterised in that the consumption of the solvent described in step (1) is: 100kg fine polytetrafluoroethylpowder powder: 20~50kg solvents;Solvent is that in ethanol, isopropanol, one or both form mixed solvent with water, and consumption of organic solvent is more than the consumption of water.
The preparation method of a kind of polytetrafluoroethylgranule granule the most as claimed in claim 1, it is characterised in that step (4) described drying is first to be warming up to 120~150 DEG C, constant temperature 10 hours, then is warming up to 250~280 DEG C, constant temperature 10 hours.
6. the preparation method of a kind of polytetrafluoroethylgranule granule as described in one of claim 1-5, it is characterised in that in step (1), the mean diameter of fine polytetrafluoroethylpowder powder is 5~50 microns.
CN201610189559.2A 2016-03-30 2016-03-30 A kind of preparation method of polytetrafluoroethylgranule granule Active CN105835251B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107552777A (en) * 2017-09-05 2018-01-09 昆山玛冀电子有限公司 A kind of powder particle composition and production technology for inductance production
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
CN109774001A (en) * 2018-11-27 2019-05-21 江西势通钙业有限公司 A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane
CN111873499A (en) * 2020-07-31 2020-11-03 德清华通新材料科技有限公司 Manufacturing process of shockproof stair board

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CN101899190A (en) * 2010-06-30 2010-12-01 上海三爱富新材料股份有限公司 Production method of polytetrafluoroethylene granular powder
CN204955175U (en) * 2015-08-26 2016-01-13 济南赛诺富隆新材料有限公司 Pre -pressing machine of polytetrafluoroethylene granule

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US4302413A (en) * 1978-11-16 1981-11-24 Rogers Corporation Process for preparing extrudable polyimide granules
CN1202184A (en) * 1995-11-09 1998-12-16 大金工业株式会社 Granulated polytetrafluorethylene for molding and process for production thereof
CN1316462A (en) * 1997-03-17 2001-10-10 大金工业株式会社 Polytetrafluorethylene granular powder containing filler
CN1923886A (en) * 2005-08-29 2007-03-07 山东东岳高分子材料有限公司 Preparation method of solvent-recoverable polytetrafluoroethylene free-flowing granulation material
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CN204955175U (en) * 2015-08-26 2016-01-13 济南赛诺富隆新材料有限公司 Pre -pressing machine of polytetrafluoroethylene granule

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107552777A (en) * 2017-09-05 2018-01-09 昆山玛冀电子有限公司 A kind of powder particle composition and production technology for inductance production
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
CN109774001A (en) * 2018-11-27 2019-05-21 江西势通钙业有限公司 A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane
CN111873499A (en) * 2020-07-31 2020-11-03 德清华通新材料科技有限公司 Manufacturing process of shockproof stair board

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