CN102875711A - Condensing washing method of polyvinylidene fluoride emulsion - Google Patents
Condensing washing method of polyvinylidene fluoride emulsion Download PDFInfo
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Abstract
The invention relates to a condensing washing method of polyvinylidene fluoride emulsion. The condensing washing method comprises the steps as follows: (1) adding water at 1 to 15 DEG C to polyvinylidene fluoride emulsion; adjusting specific gravity of emulsion to value between 1.04 and 1.18; (2) condensing the polyvinylidene fluoride emulsion obtained in an agitating mode; controlling the agitating speed to 500 to 2000 rotation per minute; completely demulsifying for 1 to 15 minutes; and (3) washing the separated polyvinylidene fluoride emulsion resin after condensing with water. According to the condensing washing method provided by the invention, the production capacity of equipment is greatly improved, water consumption is reduced, the processing period is shortened, and the benefit is brought to the scale industrial production.
Description
Technical field
The present invention relates to the aftertreatment field of polymer emulsion, particularly, relate to a kind of cohesion washing methods of polyvinylidene difluoride (PVDF) emulsion.
Background technology
Polyvinylidene difluoride (PVDF) (PVDF) has remarkable physical strength, shock-resistant, radiation resistance, water-fast and chemicals-resistant, the performance such as weather-proof, and has that piezo-electric modulus is large, refractive index is low, frequency response is wide, low resistance easily mates characteristics.Long term operation temperature-50 ~ 150 ℃, available general thermoplastics processing method processing.Its outstanding feature is that mechanical property is high, has good chemical stability.Polyvinylidene difluoride (PVDF) is by in a large number for the manufacture of various electric wires, chemical industry pipe fitting, container conduit lining, weatherability coating and film and piezoelectric film etc.
Polyvinylidene difluoride (PVDF) now industrialized polymerization process mainly is letex polymerization, and the formed emulsion of letex polymerization must be through just can further processing after the cohesion.Agglomeration process is exactly the process of a breakdown of emulsion, and the method for breakdown of emulsion mainly contains physics breakdown of emulsion and two kinds of methods of chemical demulsification, physics breakdown of emulsion such as freezing, stirring etc., and chemical demulsification is as saltouing etc.
At present the breaking method that adopts of polyvinylidene difluoride (PVDF) mainly is mechanical breakdown of emulsion, and emulsion by certain whipped form, is mutually clashed into molecule to be combined into the larger particle of volume by high speed shear and separated out from emulsion, thereby reach demulsification.Because residual various ions can have influence on the outward appearance of product in the polymerization process, so the material after breakdown of emulsion is separated out will wash, after being removed, further processes residual ion-cleaning.
Document " research of polyvinylidene difluoride (PVDF) emulsion after-treatment technology " (synthetic resins and plastics, 2005,22 (2): 35) reported the aftertreatment of polyvinylidene difluoride (PVDF) emulsion, comprised the process of breakdown of emulsion cohesion, separating, washing.Wherein the breakdown of emulsion cohesion adopts the mode that adds flocculation agent to carry out, and specifically adopts the salts such as aluminum nitrate, calcium chloride, Repone K as flocculation agent, and especially best with the flocculating result of aluminum nitrate, its massfraction is 1%; Condensation temperature remains on more than 60 ℃, and mixing speed is that the particle diameter of the resin of 100r/min(cohesion is 28 ~ 32 μ m).Wherein wash conditions is: with the high purity water washing, through 6 ~ 7 times washing, other conditions do not illustrate too much that (specific conductivity of washing mother liquor is less than or equal to 5 μ s/cm, washs 7 times; And when washing 4 times, specific conductivity is also greater than 10).The problem that document public technology exists is: the particle diameter after the cohesion is less, condenses the pvdf resin that in the pasty state, is unfavorable for next step washing, and washs 4 specific conductivity also greater than 10.
Summary of the invention
In order to overcome the problem of prior art existence, the purpose of this invention is to provide a kind of cohesion washing methods of polyvinylidene difluoride (PVDF) emulsion.
The cohesion washing methods of polyvinylidene difluoride (PVDF) emulsion provided by the invention may further comprise the steps:
(1) adding temperature in the polyvinylidene difluoride (PVDF) emulsion is 1 ~ 15 ℃ water, regulates emulsion proportion between 1.04 ~ 1.18;
(2) the polyvinylidene difluoride (PVDF) emulsion that adopts alr mode that the upper step was obtained is condensed, and mixing speed is controlled to be 500 ~ 2000 rev/mins, and the breakdown of emulsion time is 1 ~ 15min fully;
The polyvinylidene fluoride resin of (3) separating out after the cohesion washes with water.
Wherein, in the step (1), preferred 5 ~ 10 ℃ of the temperature of described water, more preferably 8 ℃.
Wherein, in the step (1), the proportion of polyvinylidene difluoride (PVDF) emulsion is preferred 1.06 ~ 1.12, and more preferably 1.08.
Wherein, in the step (2), preferred 1200 ~ 1600 rev/mins of mixing speed, more preferably 1400 rev/mins.If do not adopt such mixing speed, meeting is to separate out the particle diameter of resin very little, and following process is very inconvenient.
Wherein, because the freezing breakdown of emulsion of step (1) and the mechanical breakdown of emulsion of step (2) carry out simultaneously, the breakdown of emulsion time be that this two goes on foot breakdown of emulsion time sum, preferred 5 ~ 10min, more preferably 8min fully described in the step (2).
In the step of aforesaid method (1), if emulsion proportion less than 1.04, pool time is long, productive rate is low, and the resin particle diameter that obtains is less than normal; Emulsion proportion is higher than 1.18, and under stirring action, some emulsion can be scattered in the toner during cohesion, during washing, along with the eliminating of water, causes the waste of emulsion, reduces productive rate.When water temp was lower than 1 ℃, the emulsion particle movement rate reduced, thereby has reduced the chance of colliding between the particle, and the emulsion primary particle is reunited, and it is just little that cohesion produces the secondary particle particle diameter; When temperature was higher than 15 ℃, grain diameter influence was little to secondary particle, had prolonged on the contrary the time of breakdown of emulsion.
Wherein, in the step (3), the temperature of described water is 50 ~ 100 ℃, preferred 70 ~ 90 ℃, and more preferably 80 ℃.
Wherein, in the step (3), the number of times of washing is 2 ~ 6 times, preferred 3 ~ 4 times, and more preferably 4 times; All wash 3 ~ 10min, preferred 4 ~ 8min, more preferably 6min at every turn.
Wherein, in the step (3), the polyvinylidene fluoride resin that the upper step separates out when washing at every turn and the volume ratio of water are 1:(1.5 ~ 2).And the process of the freezing breakdown of emulsion of step (1), the volume ratio of emulsion and water does not have the ratio determined, add entry volume what, see the proportion height situation of former emulsion; If the proportion of former emulsion is high, the amount of the water that adds is just large, otherwise the amount that just adds is just few.
Wherein, in the step (3), electrical conductivity of water is less than or equal to 10 μ s/cm after the washing.
The method of the invention, described water can be used deionized water, distilled water or high purity water.Preferred deionized water, industrial production cost is lower.
The method of the invention as the polyvinylidene difluoride (PVDF) emulsion of raw material, can directly be brought usefulness, also can leave standstill at normal temperatures for some time to carry out aforesaid method again and operate.Through the emulsion that letex polymerization comes, in just polymerization out, emulsion is that higher temperature is arranged, and by leaving standstill for some time in normal temperature environment, the temperature potential of emulsion must reduce, and for adopting the Refrigerating Machinery flocculate and break emulsion, the carrying out of the low more favourable subsequent operations of temperature.
If the independent mechanical breakdown of emulsion time increases, independent freezing breakdown of emulsion not only the breakdown of emulsion cycle long, also have the energy consumption height of refrigerating process, certainly will for industrial production, greatly increase the cost of product.The machinery breakdown of emulsion is the PVDF emulsion with strong mechanical stirring, because the collision rate of PVDF particle is accelerated in the emulsion, its Efficiency Decreasing of bonding force when making the position, motor point of emulsifying agent in the emulsion be not enough to overcome collision causes the PVDF molecule to be separated from emulsion, i.e. breakdown of emulsion.Freezing breakdown of emulsion is that most emulsions produce demulsifying phenomenon after freezing, and its reason is to be to be refrigerated to after the freezing point, and water is at first separated out ice crystal, so form gradually tectum because the density of ice is lower than water.Be subject to mechanical pressure because the continuation of ice crystal increases the emulsion that is closed in below the tectum, and the electrolyte concentration in the emulsion system strengthens comparatively speaking, thereby cause high-polymer molecular to be separated out, be i.e. breakdown of emulsion.And the present invention adopts freezing and mechanical condensed phase to be combined to have reached compared with prior art, better demulsification.
The method of the invention provides is the cohesion washing methods for the formed polyvinylidene difluoride (PVDF) emulsion of letex polymerization, mechanical breakdown of emulsion and freezing breakdown of emulsion are combined, has better demulsification, median size increases greatly that (median size of the inventive method is about 200 μ m, only have about 30 μ m and other usual ways obtain), and the flocculate and break emulsion time greatly shorten (in the 15min).And further, washing process adopts hot wash, has increased electrolytical solubleness, thereby has shortened washing time, just can obtain qualified product with less washing times and water consumption.In a word, the present invention has improved the throughput of equipment greatly, reduces the consumption of water, has shortened treatment cycle, is conducive to large-scale industrial production.
Embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Other operations of not writing exactly among the present invention are added to the normal condition of this area, and employed material is the conventional material for buying from the market also.
Embodiment 1
(1) adding temperature in the 500mL polyvinylidene difluoride (PVDF) emulsion is 8 ℃ deionized water, and regulating emulsion proportion is 1.08;
(2) open stirring, mixing speed is controlled to be 1400 rev/mins, and the breakdown of emulsion time is 8min fully; The median size of PVDF emulsion is about 20 μ m before the cohesion, and the median size after the cohesion is 230 μ m;
(3) the flocculate and break emulsion polyvinylidene fluoride resin of separating out, it is 80 ℃ deionized water wash with temperature, when each washing 5min(washs at every turn, the polyvinylidene fluoride resin that the upper step separates out and deionized water volume ratio are 1:2), repetitive scrubbing 7 times, measure deionization electrical conductivity of water after the washing, be lower than 10 μ s/cm i.e. qualified (wash 4 times just up to specification), the rear PVDF of washing is white in color Powdered.
Embodiment 2
(1) adding temperature in the 500mL polyvinylidene difluoride (PVDF) emulsion is 10 ℃ deionized water, and regulating emulsion proportion is 1.06;
(2) open stirring, mixing speed is controlled to be 1600 rev/mins, and the breakdown of emulsion time is 5min fully; Condense the median size of front PVDF emulsion about 20 μ m, the median size 180 μ m after the cohesion;
(3) the flocculate and break emulsion polyvinylidene fluoride resin of separating out, it is 70 ℃ deionized water wash with temperature, when each washing 8min(washs at every turn, the polyvinylidene fluoride resin that the upper step separates out and deionized water volume ratio are 1:1.18), repetitive scrubbing 4 times, measure the rear deionization electrical conductivity of water of washing, it is namely qualified to be lower than 10 μ s/cm, and PVDF is white in color Powdered after the washing.
Embodiment 3
(1) adding temperature in the 500mL polyvinylidene difluoride (PVDF) emulsion is 5 ℃ deionized water, and regulating emulsion proportion is 1.12;
(2) open stirring, mixing speed is controlled to be 1200 rev/mins, and the breakdown of emulsion time is 10min fully; Condense the median size of front PVDF emulsion about 20 μ m, the median size 200 μ m after the cohesion;
(3) the flocculate and break emulsion polyvinylidene fluoride resin of separating out, it is 90 ℃ deionized water wash with temperature, when each washing 4min(washs at every turn, the polyvinylidene fluoride resin that the upper step separates out and deionized water volume ratio are 1:6), repetitive scrubbing 4 times, measure the rear deionization electrical conductivity of water of washing, it is namely qualified to be lower than 10 μ s/cm, and PVDF is white in color Powdered after the washing.
Embodiment 4
(1) adding temperature in the 500mL polyvinylidene difluoride (PVDF) emulsion is 15 ℃ deionized water, and regulating emulsion proportion is 1.18;
(2) open stirring, mixing speed is controlled to be 500 rev/mins, and the breakdown of emulsion time is 15min fully; Condense the median size of front PVDF emulsion about 20 μ m, the median size 210 μ m after the cohesion;
(3) the flocculate and break emulsion polyvinylidene fluoride resin of separating out, it is 50 ℃ deionized water wash with temperature, when each washing 10min(washs at every turn, the polyvinylidene fluoride resin that the upper step separates out and deionized water volume ratio are 1:1.5), repetitive scrubbing 3 times, measure the rear deionization electrical conductivity of water of washing, it is namely qualified to be lower than 10 μ s/cm, and PVDF is white in color Powdered after the washing.
Embodiment 5
(1) adding temperature in the 500mL polyvinylidene difluoride (PVDF) emulsion is 1 ℃ deionized water, and regulating emulsion proportion is 1.04;
(2) open stirring, mixing speed is controlled to be 2000 rev/mins, and the breakdown of emulsion time is 1min fully; Condense the median size of front PVDF emulsion about 20 μ m, the median size 170 μ m after the cohesion;
(3) the flocculate and break emulsion polyvinylidene fluoride resin of separating out, it is 100 ℃ deionized water wash with temperature, when each washing 3min(washs at every turn, the polyvinylidene fluoride resin that the upper step separates out and deionized water volume ratio are 1:2), repetitive scrubbing 4 times, measure the rear deionization electrical conductivity of water of washing, it is namely qualified to be lower than 10 μ s/cm, and PVDF is white in color Powdered after the washing.
Comparative Examples
Other conditions are experiment condition 1 in the following table with embodiment 1(embodiment 1 corresponding group), difference be all use normal-temperature water (25 ℃) to carry out the washing of the cohesion of step (1) (the polyvinylidene fluoride resin volume behind the breakdown of emulsion is 250mL) and step (3) (each washing is added deionized water and is 500mL, each washing time is 5min), group is the experiment condition 2 in the following table.
Comparing result see the following form (sensing range in the form is specific conductivity≤30 μ s/cm):
Can find out from the as a result comparative analysis of upper table, with breakdown of emulsion time of cold water than shortened for 44% time with normal-temperature water.And, just qualified with hot deionized water washing 4 times during washing, all do not have for 7 times qualifiedly and washed with normal-temperature water, bath water is over half than Duo with hot deionized water, and washs afterwards that PVDF is little yellow.Compare by breakdown of emulsion time and bath water amount, present method has shortened the breakdown of emulsion time, has reduced the bath water amount, thereby has greatly improved the throughput of equipment, is conducive to suitability for industrialized production.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the cohesion washing methods of a polyvinylidene difluoride (PVDF) emulsion may further comprise the steps:
(1) adding temperature in the polyvinylidene difluoride (PVDF) emulsion is 1 ~ 15 ℃ water, regulates emulsion proportion between 1.04 ~ 1.18;
(2) the polyvinylidene difluoride (PVDF) emulsion that adopts alr mode that the upper step was obtained is condensed, and mixing speed is controlled to be 500 ~ 2000 rev/mins, and the breakdown of emulsion time is 1 ~ 15min fully;
The polyvinylidene fluoride resin of (3) separating out after the cohesion washes with water.
2. method according to claim 1 is characterized in that, in the step (1), the temperature of described water is 5 ~ 10 ℃, preferred 8 ℃.
3. method according to claim 1 is characterized in that, in the step (1), the proportion of polyvinylidene difluoride (PVDF) emulsion is 1.06 ~ 1.12, preferred 1.08.
4. the described method of any one is characterized in that according to claim 1 ~ 3, and in the step (2), mixing speed is 1200 ~ 1600 rev/mins, preferred 1400 rev/mins.
5. the described method of any one is characterized in that according to claim 1 ~ 3, and in the step (2), the described complete breakdown of emulsion time is 5 ~ 10min, preferred 8min.
6. the described method of any one is characterized in that according to claim 1 ~ 5, and in the step (3), the temperature of water is 50 ~ 100 ℃, preferred 70 ~ 90 ℃.
7. the described method of any one is characterized in that according to claim 1 ~ 5, and in the step (3), the number of times of washing is 2 ~ 6 times, preferred 3 ~ 4 times; All wash 3 ~ 10min, preferred 4 ~ 8min at every turn.
8. method according to claim 7 is characterized in that, in the step (3), when washing, the polyvinylidene fluoride resin that the upper step separates out and the volume ratio of water are 1:(1.5 ~ 2 at every turn).
9. the described method of any one is characterized in that according to claim 1 ~ 8, and in the step (3), electrical conductivity of water is less than or equal to 10 μ s/cm after the washing.
10. method according to claim 1 is characterized in that, described water is deionized water, distilled water or high purity water.
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| CN109320634A (en) * | 2017-07-31 | 2019-02-12 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN110016098A (en) * | 2019-02-25 | 2019-07-16 | 聊城氟尔新材料科技有限公司 | A kind of perfluoroethylene-propylene production cohesion wash mill |
| CN110078846A (en) * | 2019-04-22 | 2019-08-02 | 中昊晨光化工研究院有限公司 | A kind of post-processing approach of polyvinylidene fluoride emulsion |
| CN110317286A (en) * | 2018-03-30 | 2019-10-11 | 浙江蓝天环保高科技股份有限公司 | A method of improving polyvinylidene fluoride resin degree of purity |
| CN111440255A (en) * | 2020-03-26 | 2020-07-24 | 东莞东阳光科研发有限公司 | Post-treatment method of fluorine-containing resin emulsion and fluorine-containing resin |
| CN113861312A (en) * | 2021-11-23 | 2021-12-31 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of powdered fluororubber |
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| CN104530265A (en) * | 2014-12-18 | 2015-04-22 | 中昊晨光化工研究院有限公司 | Fluorine-containing polymer powder and preparation method thereof |
| CN104530265B (en) * | 2014-12-18 | 2017-07-11 | 中昊晨光化工研究院有限公司 | A kind of fluoropolymer powder and preparation method thereof |
| CN109320634A (en) * | 2017-07-31 | 2019-02-12 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN109320634B (en) * | 2017-07-31 | 2019-11-22 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN110317286A (en) * | 2018-03-30 | 2019-10-11 | 浙江蓝天环保高科技股份有限公司 | A method of improving polyvinylidene fluoride resin degree of purity |
| CN110016098A (en) * | 2019-02-25 | 2019-07-16 | 聊城氟尔新材料科技有限公司 | A kind of perfluoroethylene-propylene production cohesion wash mill |
| CN110078846A (en) * | 2019-04-22 | 2019-08-02 | 中昊晨光化工研究院有限公司 | A kind of post-processing approach of polyvinylidene fluoride emulsion |
| CN111440255A (en) * | 2020-03-26 | 2020-07-24 | 东莞东阳光科研发有限公司 | Post-treatment method of fluorine-containing resin emulsion and fluorine-containing resin |
| WO2022262156A1 (en) | 2021-06-16 | 2022-12-22 | 浙江巨圣氟化学有限公司 | Method for improving coagulating effect of fluororubber emulsion |
| CN113861312A (en) * | 2021-11-23 | 2021-12-31 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of powdered fluororubber |
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