CN102775617B - Preparation method of colored polytetrafluoroethylene resin - Google Patents
Preparation method of colored polytetrafluoroethylene resin Download PDFInfo
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Abstract
The invention discloses a preparation method of a colored polytetrafluoroethylene resin, which comprises the following steps: adding 500 parts of deionized water, 145 parts of tetrafluoroethylene monomer, 0.1-0.18 part of activating agent, 15-22 parts of emulsifier, 0.02-0.06 part of initiator and 15-20 parts of stabilizer into a reaction kettle, carrying out polymerization reaction at 50-100 DEG C under the pressure of 1.0-3.0Mpa, finishing the reaction when the pressure of the reaction kettle is 0.3Mpa, standing, cooling, discharging, and separating out the stabilizer; adding deionized water into the material without the stabilizer until the solid content is 10-20%; and while stirring, adding ammonia water to regulate the pH value of the material to 8-10, adding 0.5-1.5 parts of pigment, condensing at 15-35 DEG C at the rotation speed of 80-100 r/min for 8-10 minutes, separating out the supernatant condensate, and drying the supernatant condensate at 110-200 DEG C for 7-12 hours to obtain the colored polytetrafluoroethylene resin. The invention has the advantages of simple technique, good product quality, low cost, energy saving and environmental protection.
Description
Technical field
The present invention relates to the preparation method of teflon resin, particularly a kind of preparation method of colorful Teflon resin.
Background technology
Polytetrafluoroethylene (PTFE) is the high crystallinity polymer of tetrafluoroethylene monomer, is the thermoplastics that a kind of white has wax-like sensation.In PTFE; fluorine atom instead of the hydrogen atom in polyethylene; make carbon carbon bond by poly plane, that wide-spread tortuous conformation is torqued into PTFE gradually helical conformation; this helical conformation is just in time enclosed in PTFE and is subject to outside the carbon chain backbone of chemical attack; thus define the protective layer of completely " fluoro " closely; make PTFE show good mechanical property, electrical property, chemical resistance, weather resisteant and non-viscosity and oilness, be synthesized material circle and be described as " King ".
In application aspect, PTFE is the preferred material of the applied corrosion resistant lining of anticorrosion pipeline, pipe fitting, corrugated tube, the pump housing, valve, still, groove, tower and various standard equipment.In addition, use very extensive as sealing material, lubricant in industries such as machinery, petrochemical industry, communications and transportation, medicine, food, light industry, weaving, buildings.According to after the process of PTFE film, there is selective penetrated property, can be used as parting material, selectively through gas or liquid, its porous-film also for gas-liquid separation and Liquid liquid Separation, and for filtering corrosive liquid.Along with the continuous expansion of the market requirement, single white resin can not tackle the market requirement, and the exploitation of color resin is the color that can provide more alternative processed goods to market.
Along with progressively widening of colorful Teflon range of application, the demand of colorful Teflon is increased day by day, but be only limitted to carry out color processing technique in tetrafluoroethylene machine-shaping process in disclosed technological method at present, it is uneven that the product obtained also exists colo(u)rant dispersion, the unstable properties such as anticorrosive, high temperature resistant, dust from flying during pigment and resin mixing, the shortcomings such as production environment is severe, significantly limit the application and development of colorful Teflon.
As China Patent Publication No. CN101696753 A, publication date on April 21st, 2010, denomination of invention: with white polytetrafluoroethylpipe pipe and the manufacture method thereof of colored sign line, this application case discloses a kind of white polytetrafluoroethylpipe pipe with colored sign line and manufacture method thereof, the markings of different colours can be utilized to be distinguished completely by white polytetrafluoroethylpipe pipe, like this when concentrated use many white polytetrafluoroethylpipe pipes carry different fluid mediums, operator can not only observe the changing conditions of every bar tubing inside, and can also effectively distinguish different types of fluid medium according to colored sign line.Its weak point is the method is in tetrafluoroethylene machine-shaping process, add pigment slaking and obtain, and technique is loaded down with trivial details, the three wastes are many, cost is high, efficiency is low.
And for example China Patent Publication No. CN87103955 A, publication date on December 14th, 1988, denomination of invention: colored masterbatch of fluor-oplastics and preparation method thereof, this application case discloses the preparation method of the colored masterbatch of a kind of fluoro-resin, first add wet pigment, after fluorine-containing dispersant, fully mix with fluoro-resin again, wet feed at high temperature sinters, cut into slices, extruding pelletization obtains product, weak point is the more difficult control of the ratio of tinting material in resin, and the interpolation of tinting material, there is disadvantageous effect to the performance such as tensile strength, elongation at break of goods.
For another example China Patent Publication No. CN101597379A, publication date on December 9th, 2009, denomination of invention: the making method of the colored raw material band of winding and sintering tetrafluoroethylene, this application case discloses the making method of the colored raw material band of a kind of winding and sintering tetrafluoroethylene, its making step is: polytetrafluoroethyldispersion dispersion resin is through sieving, the pigment accounting for resin quality 1 ~ 5% is added in resin after sieving, then propellant mixing is added, 24 hours post curing treatment placed by mixed raw material, then pre-molding blank is extruded, prolong through two roll-ins, by removing propellant, through shaping process, cut again, rolling, the colored raw material band of final obtained winding and sintering tetrafluoroethylene.Weak point is that pigment disperses the mechanical propertys such as uneven, product tensile strength, elongation at break unstable in teflon resin.
Summary of the invention
The present invention is directed to the deficiencies in the prior art part, provide that a kind of technique is simple, good product quality, cost are low, the preparation method of the colorful Teflon resin of energy-conserving and environment-protective.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of colorful Teflon resin, deionized water 500 parts, tetrafluoroethylene monomer 145 parts, activator 0.1-0.18 part, emulsifying agent 15-22 part, initiator 0.02-0.06 part, stablizer 15-20 part are dropped into reactor, it is 50 ~ 100 DEG C in temperature of reaction, pressure is carry out polyreaction under the condition of 1.0 ~ 3.0 Mpa, when being 0.3Mpa to reactor pressure, terminate reaction, standing, cooling discharging, separating stable agent; Then in the material after separating stable agent, add deionized water makes solid content be after 10% ~ 20%, under agitation adding ammoniacal liquor regulates material pH value to be 8 ~ 10, add 0.5-1.5 part pigment again, 8 ~ 10min is condensed at 80-100r/min rotating speed and 15-35 DEG C, isolate upper strata condensation product, within 7 ~ 12 hours, namely obtain colorful Teflon resin by dry at 110 ~ 200 DEG C for upper strata condensation product.
Further:
Described activator is acetic acid or hydrochloric acid.
Described emulsifying agent is ammonium perfluorocaprylate or perfluoro octyl sulfonic acid potassium.
Described initiator is peroxysuccinic acid or ammonium persulphate.
Described stablizer is paraffin or chlorofluorocarbon oil.
Described temperature of reaction is 70-90 DEG C, and pressure is 2.0-2.5 Mpa.
Described solid content is 12% ~ 15%.
Described pigment is pigment dyestuff.
Described pigment is azo pigment.
Described drying temperature is 130-180 DEG C, and time of drying is 8 ~ 11 hours.
Activator can be supplied to polymerization system initial polymerization speed faster.But activator adds too much, polymerization rate is very fast, and be difficult to control, activator adds very little, and polymerization original speed is comparatively slow, and affect the W-response time, therefore in the present invention, the number that adds of activator is 0.1-0.18 part.Activator can select mineral acid and organic acid, example hydrochloric acid, acetic acid, oxalic acid etc., preferred hydrochloric acid or acetic acid.
The emulsifying agent surface tension that can reduce between material makes material more easily dissolve each other.But emulsifying agent adds too much, increase cost, add very little, can cause the serious breakdown of emulsion of emulsion, cause a large amount of consumption after reaction, therefore in the present invention, the number that adds of emulsifying agent is 15-22 part.Emulsifying agent can select perfluorooctanoic acid salt, perfluorinated sulfonate, as ammonium perfluorocaprylate, Sodium perfluorooctanoate, perfluorobutyl potassium, perfluoro hexyl potassium sulfonate, perfluoro octyl sulfonic acid potassium, is preferably ammonium perfluorocaprylate or perfluoro octyl sulfonic acid potassium.
Initiator can provide the free radical of chain starting reaction, can initiated polymerization.But initiator adds too much, reaction is too fast, and temperature, pressure is difficult to regulation and control, and affects the quality of resin, adds very little, and reaction is difficult to carry out, and therefore in the present invention, the number that adds of initiator is 0.02-0.06 part.Initiator can select alkyl peroxide, persulphate, azo compound, alkyl peroxide thing, as peroxidation two acyl, ammonium persulphate, Diisopropyl azodicarboxylate, peroxysuccinic acid, hydrogen peroxide etc., be preferably peroxysuccinic acid or ammonium persulphate.
Stablizer can improve the thermostability of resin, prevent the generation of condensation product.But stablizer adds too much, increase post-processing difficulty, also easily bring in product, affect quality product, add very little, then polymerization system poor stability, easily produces condensation product, and therefore in the present invention, the number that adds of stablizer is 15-20 part.Stablizer preferably selects paraffin or chlorofluorocarbon oil.
Temperature of reaction has impact to speed of response.Speed of response is accelerated with the rising of temperature of reaction, but temperature of reaction is too high, and heat of polymerization is comparatively large, and it is difficult to control, and temperature is too low, and reaction is difficult to carry out, and the temperature of reaction therefore in the present invention is 50-100 DEG C, is preferably 70-90 DEG C.
Reaction pressure also has impact to speed of response.Speed of response is accelerated with the rising of reaction pressure, but pressure is too high, high to equipment requirements, increase input cost, pressure is too low, and the solubleness of tetrafluoroethylene in water is lower, speed of response is slow, and the reaction pressure therefore in the present invention is 1.0 ~ 3.0MPa, is preferably 2.0 ~ 2.5MPa.
Solid content has impact to the size of particle after condensation degree and cohesion, and solid content is too high, then particle is comparatively large, and solid content is too low, then particle is less, and therefore in the present invention, solid content is selected at 10%-20%, preferred 12-15%.
Pigment can select pigment dyestuff and mineral dye; Because pigment dyestuff good water solubility, can well mix with polymeric solution, strong coloring force, so preferably select pigment dyestuff, as azo pigment, phthalocyanine pigment, triaryl methane pigment, polycyclic pigment, preferred azo pigment, all can commercially availablely obtain with paint, selects the azo pigment such as the red superfine aqueous color sizing of the N-LF black superfine aqueous color sizing of Shanghai Xu Hua trade Co., Ltd levanyl series, BB-LF, the blue superfine aqueous color sizing of G-LF, the yellow superfine aqueous color sizing of GN-LF in the present invention.
Pigment add-on is very large on color of resin impact, adds that resin can be made too much to produce is painted uneven etc., adds very little, can not meet chromaticity requirements, so in the present invention, pigment adds number is 0.5-1.5 part.
Mixing speed has impact to colorful Teflon resin quality.Rotating speed is faster, is more conducive to breakdown of emulsion, but speed is too fast, then equipment can vibrate, and is unfavorable for producing, so stirring velocity controls at 80-100r/min in the present invention.
Need the breakdown of emulsion environment providing an acid base imbalance to material during cohesion, therefore material pH value can produce larger impact to demulsification.PH value is too low, and impact cohesion is spent completely, and pH value is too high, and flocculating result can not significantly increase, and the pH value therefore in the present invention is 8 ~ 10.
Condensation temperature and the completely degree of time on cohesion have impact.Temperature is too high, and condensation degree reduces, and there will be the resin that particle is less, temperature is too low, and energy consumption is large, uneconomical; Pool time is oversize, lengthens working hours, too short, can not condense completely, and the condensation temperature therefore in the present invention is 15-35 DEG C, and pool time is 8-10min.
There are impact drying temperature and time on resin quality.Temperature is too high or the time is oversize, serious to the infringement of electric installation, and pigment is unstable easily to be decomposed, and temperature is too low or the time is too short, and resin aqueous amount is defective, so the drying temperature of resin is 110 ~ 200 DEG C in the present invention, is preferably 130 ~ 180 DEG C; Time of drying is 7 ~ 12 hours, is preferably 8 ~ 11 hours.
The present invention has that technique is simple, good product quality, cost are low, the advantage of energy-conserving and environment-protective, the tetrafluoroethylene product produced both had remained the excellent mechanical property of the tensile strength, elongation at break etc. of original white resin, met again the needs that resin treatment becomes the finished product of shades of colour and color and luster.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples.
embodiment 1
Be in the autoclave of 1L at volume, add 500g deionized water, 0.15g acetic acid, 15g ammonium perfluorocaprylate, 15g paraffin, then closed reactor, reactor is found time, replacement operator, and carry out oxygen level test, when oxygen level≤20ppm in reactor is qualified.By still temperature rise to 50 DEG C after oxygen level is qualified, and drop into TFE monomer to still pressure 2.0Mpa in reactor after, add 0.02g initiator peroxysuccinic acid by high-pressure pump and start reaction, continue in reaction process to pass into TFE monomer to maintain pressure at 2.0Mpa, when TFE monomer add-on is 145g, stop adding TFE monomer in reactor, overbottom pressure reaction is to 0.3 Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Leave standstill 5 minutes, open blow-off valve, cooling discharge, isolate paraffin; Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 15%; Again cohesion medial launder material is put in collection surface, open and stir, add ammoniacal liquor and regulate material pH value to be 9, condense 10min at 80r/min rotating speed and 30 DEG C after, isolate upper strata condensation product; Upper strata condensation product is obtained white resin 140g after dry 8.5 hours at 170 DEG C.
embodiment 2
Be in the autoclave of 1L at volume, add 500g deionized water, 0.13g acetic acid, 17g perfluoro octyl sulfonic acid potassium, 16g chlorofluorocarbon oil, then closed reactor, reactor is found time, replacement operator, and carry out oxygen level test, when oxygen level≤20ppm in reactor is qualified.By still temperature rise to 70 DEG C after oxygen level is qualified, and drop into TFE monomer to still pressure 1.8Mpa in reactor after, add 0.03g initiator ammonium persulfate by high-pressure pump and start reaction, continue in reaction process to pass into TFE monomer to maintain pressure at 1.8Mpa, when TFE monomer add-on is 145g, stop adding TFE monomer in reactor, overbottom pressure reaction is to 0.3 Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Leave standstill 5 minutes, open blow-off valve, cooling discharge, isolate chlorofluorocarbon oil; Then the material after separate fluorine fluorocarbon oil is put into cohesion medial launder, adds deionized water and make solid content be 13%; Again cohesion medial launder material is put in collection surface, open and stir, adding ammoniacal liquor regulates material pH value to be 9, add 0.5g levanyl series N-LF black superfine aqueous color sizing (purchased from Shanghai Xu Hua trade Co., Ltd) again, condense 9min at 80r/min rotating speed and 20 DEG C after, isolate upper strata condensation product; Black teflon resin 140 grams within 9 hours, is obtained, water content 0.02% by dry at 150 DEG C for upper strata condensation product.
embodiment 3
Be in the autoclave of 1L at volume, add 500g deionized water, 0.4g mass percentage concentration is the hydrochloric acid of 35%, 19g ammonium perfluorocaprylate, 18g paraffin, then closed reactor, find time to reactor, replacement operator, and carry out oxygen level test, when oxygen level≤20ppm in reactor is qualified.By still temperature rise to 60 DEG C after oxygen level is qualified, and drop into TFE monomer to still pressure 2.5Mpa in reactor after, add 0.06g initiator peroxysuccinic acid by high-pressure pump and start reaction, continue in reaction process to pass into TFE monomer to maintain pressure at 2.5Mpa, when TFE monomer add-on is 145g, stop adding TFE monomer in reactor, overbottom pressure reaction is to 0.3 Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Leave standstill 5 minutes, open blow-off valve, cooling discharge, isolate paraffin; Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 14%; Again cohesion medial launder material is put into collection surface, open and stir, adding ammoniacal liquor regulates material pH value to be 10, add the red superfine aqueous color sizing (purchased from Shanghai Xu Hua trade Co., Ltd) of 0.8g levanyl series BB-LF again, at 90r/min rotating speed and 25 DEG C, condense 10min, isolate upper strata condensation product; By upper strata condensation product at 130 DEG C dry 11 hours, obtain red teflon resin 142 grams, water content was 0.02%.
embodiment 4
Be in the autoclave of 1L at volume, add 500g deionized water, 0.10g acetic acid, 21g perfluoro octyl sulfonic acid potassium, 19g paraffin, then closed reactor, reactor is found time, replacement operator, and carry out oxygen level test, when oxygen level≤20ppm in reactor is qualified.By still temperature rise to 80 DEG C after oxygen level is qualified, and drop into TFE monomer to still pressure 2.1Mpa in reactor after, add 0.05g initiator peroxysuccinic acid by high-pressure pump and start reaction, continue in reaction process to pass into TFE monomer to maintain pressure at 2.1Mpa, when TFE monomer add-on is 145g, stop adding TFE monomer in reactor, overbottom pressure reaction is to 0.3 Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Leave standstill 5 minutes, open blow-off valve, cooling discharge, isolate paraffin; Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 12%; Again cohesion medial launder material is put into collection surface, open and stir, adding ammoniacal liquor regulates material pH value to be 8, add the blue superfine aqueous color sizing (purchased from Shanghai Xu Hua trade Co., Ltd) of 1.0g levanyl series G-LF again, at 100r/min rotating speed and 15 DEG C, condense 8min, isolate upper strata condensation product; By upper strata condensation product at 180 DEG C dry 8 hours, obtain blue teflon resin 139 grams, water content was 0.02%.
embodiment 5
Be in the autoclave of 1L at volume, add 500g deionized water, 0.5g mass percentage concentration is the hydrochloric acid of 35%, 22g ammonium perfluorocaprylate, 20g chlorofluorocarbon oil, then closed reactor, find time to reactor, replacement operator, and carry out oxygen level test, when oxygen level≤20ppm in reactor is qualified.By still temperature rise to 100 DEG C after oxygen level is qualified, and in reactor, drop into TFE monomer press 1.5Mpa to still, add 0.05g initiator peroxysuccinic acid by high-pressure pump and start reaction, continue in reaction process to pass into TFE monomer to maintain pressure at 1.5Mpa, when TFE monomer add-on is 145g, stop adding TFE monomer in reactor, overbottom pressure reaction is to 0.3 Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Leave standstill 5 minutes, open blow-off valve, cooling discharge, isolate chlorofluorocarbon oil; Then the material after separate fluorine fluorocarbon oil is put into cohesion medial launder, adds deionized water and make solid content be 12%; Again cohesion medial launder material is put into collection surface, open stirring, adding ammoniacal liquor regulates material pH value to be 10, add the yellow superfine aqueous color sizing (purchased from Shanghai Xu Hua trade Co., Ltd) of 1.5g levanyl series GN-LF again, at 95r/min rotating speed and 35 DEG C, condense 10min, isolate upper strata condensation product; Drying 9.5 hours at 145 DEG C, obtain yellow teflon resin 141 grams, water content is 0.02%.
comparative example 1:
To in the white resin obtained according to embodiment 1 polymerization formula and reaction conditions, add wet pigment, 17 grams of dispersion agent ammonium perfluorocaprylates of 1.0 grams of cadmium reds fully to mix, wet feed at high temperature sinters, cut into slices, extruding pelletization, and obtained red teflon resin masterbatch 138 grams, water content is 0.02%.
comparative example 2:
To in the white resin obtained according to embodiment 1 polymerization formula and reaction conditions, add wet pigment, 20 grams of dispersion agent perfluoro octyl sulfonic acid potassium of 0.9 gram of chrome yellow fully to mix, wet feed at high temperature sinters, cut into slices, extruding pelletization, obtained yellow teflon resin masterbatch 140 grams, water content is 0.02%.
The mensuration of the colorful Teflon resin physical and mechanical properties that embodiment 1 ~ 5 and comparative example 1 ~ 2 obtain, in table 1, measures and presses GB7136-86 execution:
Claims (10)
1. the preparation method of a colorful Teflon resin, deionized water 500 parts, tetrafluoroethylene monomer 145 parts, activator 0.1-0.18 part, emulsifying agent 15-22 part, initiator 0.02-0.06 part, stablizer 15-20 part are dropped into reactor, it is 50 ~ 100 DEG C in temperature of reaction, pressure is carry out polyreaction under the condition of 1.0 ~ 3.0 Mpa, when being 0.3Mpa to reactor pressure, terminate reaction, standing, cooling discharging, separating stable agent; Then in the material after separating stable agent, add deionized water makes solid content be after 10% ~ 20%, under agitation adding ammoniacal liquor regulates material pH value to be 8 ~ 10, add 0.5-1.5 part pigment again, 8 ~ 10min is condensed at 80-100r/min rotating speed and 15-35 DEG C, isolate upper strata condensation product, within 7 ~ 12 hours, namely obtain colorful Teflon resin by dry at 110 ~ 200 DEG C for upper strata condensation product.
2. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described activator is acetic acid or hydrochloric acid.
3. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described emulsifying agent is ammonium perfluorocaprylate or perfluoro octyl sulfonic acid potassium.
4. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described initiator is peroxysuccinic acid or ammonium persulphate.
5. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described stablizer is paraffin or chlorofluorocarbon oil.
6. the preparation method of colorful Teflon resin according to claim 1, it is characterized in that described temperature of reaction is 70-90 DEG C, pressure is 2.0-2.5 Mpa.
7. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described solid content is 12% ~ 15%.
8. the preparation method of colorful Teflon resin according to claim 1, is characterized in that described pigment is pigment dyestuff.
9. the preparation method of colorful Teflon resin according to claim 8, is characterized in that described pigment is azo pigment.
10. the preparation method of colorful Teflon resin according to claim 1, it is characterized in that described drying temperature is 130-180 DEG C, time of drying is 8 ~ 11 hours.
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| CN104403035B (en) * | 2014-11-26 | 2016-08-24 | 浙江巨圣氟化学有限公司 | A kind of preparation method of politef dispersion emulsion |
| CN110790956B (en) * | 2019-11-01 | 2022-06-10 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of superfine fluororesin powder |
| CN112426996A (en) * | 2020-11-30 | 2021-03-02 | 德清县宝华氟塑料工贸有限公司 | Paraffin separator for polytetrafluoroethylene production |
| CN113968924A (en) * | 2021-10-21 | 2022-01-25 | 安徽元琛环保科技股份有限公司 | Preparation method of denitration catalyst micro powder in-situ filling modified PTFE dispersion resin |
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| CN1463996A (en) * | 2002-06-03 | 2003-12-31 | 中昊晨光化工研究院 | Process for producing medium compression ratio perfluoroethylene dispersing resin |
| CN1594381A (en) * | 2004-06-25 | 2005-03-16 | 吉林大学 | Fluoropolymer modified polyacrylate dispersion and its preparation and use |
| CN1882617A (en) * | 2003-11-17 | 2006-12-20 | 3M创新有限公司 | Aqueous dispersions of polytetrafluoroethylene having a low amount of fluorinated surfactant |
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| CN1463996A (en) * | 2002-06-03 | 2003-12-31 | 中昊晨光化工研究院 | Process for producing medium compression ratio perfluoroethylene dispersing resin |
| CN1882617A (en) * | 2003-11-17 | 2006-12-20 | 3M创新有限公司 | Aqueous dispersions of polytetrafluoroethylene having a low amount of fluorinated surfactant |
| CN1594381A (en) * | 2004-06-25 | 2005-03-16 | 吉林大学 | Fluoropolymer modified polyacrylate dispersion and its preparation and use |
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