CN103172863A - Method for improving washing and separating efficiency of polyphenylene sulfide particles - Google Patents
Method for improving washing and separating efficiency of polyphenylene sulfide particles Download PDFInfo
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- CN103172863A CN103172863A CN2013101174059A CN201310117405A CN103172863A CN 103172863 A CN103172863 A CN 103172863A CN 2013101174059 A CN2013101174059 A CN 2013101174059A CN 201310117405 A CN201310117405 A CN 201310117405A CN 103172863 A CN103172863 A CN 103172863A
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Abstract
The invention relates to a method for improving washing and separating efficiency of polyphenylene sulfide particles. The method is mainly characterized in that a washing machine which is partitioned into a washing cavity and a collecting cavity by a stainless steel sintering filter plate and is provided with a stirring device is used for washing. The method mainly comprises the following steps of: putting the polyphenylene sulfide particles to be washed into the washing cavity; adding a washing agent to ensure that the washing agent is over washed matters; taking hot water as a medium, and sufficiently stirring to ensure that the washed matters are uniformly mixed with the washing agent, so that microparticles in polyphenylene sulfide to be washed are separated from surfaces of large particles and are isolated and collected into the collecting cavity in time; discharging the washing agent containing the microparticles by a drain valve to finish once washing; and adding the new washing agent to repeat once or more washing till qualified washing is finished, and dropping a kettle and turning over for discharge. By means of the method, microparticles are not easy to arise and cover the large polyphenylene sulfide particles, so that possible loss of a target product in the transfer process can be avoided, and the manpower consumption is reduced.
Description
Technical field
The present invention relates to a kind of washing methods, particularly a kind of method that improves the washing of polyphenylene sulfide particle, separation efficiency.
Background technology
In general for the solid particulate of drying, can separate varigrained particulate matter by sieving, can be by filtering solid filtering out for the solid in liquid phase.But when having the particulate matter of different-grain diameter in solution, or when particulate matter surface moisture, viscous, when the particulate matter of small (setting particle diameter less than certain) is adsorbed on large particulate matter surface, allow the particulate matter of different-grain diameter separately just seem more difficult.
Traditional method is to adopt suitable solvent or medium, under the condition that stirs, the molecule of particulate matter surface adsorption is temporarily separated, but when stirring one stops, preparing filtering, the molecule that is temporarily separated can precipitate again, be adsorbed on oarse-grained surface again, cause the poor effect of washing, separating, need to obtain corresponding effect by repeatedly washing, constantly dilution, this has just increased the number of times that washs, and has increased the consumption of washing composition.
At synthetic macromolecular compound, such as during polyphenylene sulfide, polymer substance can form the particulate matter of different-grain diameter because of the difference of chaining length.Difference along with the particulate matter particle diameter, also can cause they physics, the chemistry performance different, for the performance that makes the product that obtains convergent as far as possible, need to wash product with washing composition etc., and wish in washing, can also in passing the particulate matter of different-grain diameter separately, after washing is over, can also easily washing particulate matter well be taken out.
The english abbreviation of polyphenylene sulfide is PPS, is a kind of high performance thermoplastic resin, has that physical strength is high, high temperature resistant, an advantage such as chemical resistance corrosion, difficult combustion, Heat stability is good, electrical property are good.All be widely used at electronics, automobile, machinery and chemical field.
For exist not enough of existing conventional washing plant with to the actual requirement of particulate matter washing effect, consider to research and develop a kind of raising particulate matter, particularly polyphenylene sulfide particle, the method for washing, separation efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that improves the washing of polyphenylene sulfide particle, separation efficiency, when the polyphenylene sulfide particle of washing different-grain diameter, not only can wash the liquid of the viscous of polyphenylene sulfide particle surface absorption off, and the molecule that large particle surface adheres in time can be separated, improve washing, the separation efficiency of polyphenylene sulfide particle, and avoid possible loss in purpose product transfer process, reduce the consumption of manpower.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of method that improves the washing of polyphenylene sulfide particle, separation efficiency, be mainly and adopt the washing machine that is separated into washing cavities and collecting chamber and has a whipping appts by stainless steel sintering filter plate to wash, the collecting chamber bottom arranges bleed valve, the washing cavities top arranges the kettle cover of sealing, the condensation reflux unit of charging opening and washing composition is set on kettle cover, and its innovative point is that described method mainly comprises the following steps:
The polyphenylene sulfide particle that a) will wash is placed in the washing cavities of washing machine;
B) first add acetone as washing composition, cover the polyphenylene sulfide particle that will wash;
C) washing composition is heated as heating medium with the hot water of 48～55 ℃, adopt the stainless steel sintering filter plate of setting the order number; Whipping appts by washing machine stirs polyphenylene sulfide particle and the washing composition that will wash fully, makes the particle separation of different-grain diameter; In the particle of separating less than set molecule that order counts stainless steel sintering filter plate corresponding aperture because of density greater than washing composition density, pass stainless steel sintering filter plate from washing cavities, isolated in time, collected in collecting chamber;
D) washing finishes, and after stopping stirring 10 minutes, opens bleed valve, emits the washing composition that contains molecule, and the polyphenylene sulfide particle that wash is stayed in washing cavities, then closes bleed valve;
E) adopt successively respectively tap water, tap water to add washing cavities as washing composition, repeat above-mentioned steps c)～d), in order to dissolve, wash away the sodium chloride particle of by-product;
F) adopting successively respectively mass concentration is that 0.1%～0.5% acetic acid solution, distilled water and distilled water add washing cavities as washing composition, repeats above-mentioned steps c)～d) complete to washing;
G) kettle and kettle cover are separated, adopt the lifting device of washing machine to take out the good polyphenylene sulfide particle of washing in conjunction with turning device, the polyphenylene sulfide particle is placed in dryer, oven dry is 8 hours at the temperature of 110 ± 5 ℃, after cool to room temperature, obtain the larger polyphenylene sulfide particle of granularity in loft drier.
Further, the housing of the washing cavities of described washing machine and collecting chamber adopts and is welded to connect.
The invention has the advantages that:
1) separate with stainless steel sintering filter plate between washing cavities and collecting chamber, make when washing be washed the molecule that agent temporarily separates and pass stainless steel sintering filter plate greatly because of density, in time be collected in collecting chamber.Owing to there is no agitating vane in collecting chamber, liquid does not wherein have the washing composition in washing cavities to move so severely, these sediments just are not easy to rise, cover on the polyphenylene sulfide macrobead (purpose product) that has separated molecule, can improve washing, the separation efficiency of polyphenylene sulfide particle.
2) when certain washing end, when opening the bleed valve of collecting chamber bottom, molecule can be discharged from together in company with washing composition, after closing bleed valve, need not take out the polyphenylene sulfide particle that will wash, add fresh washing composition just can begin the washing of next time, thereby not only can avoid the possible loss in transfer process of purpose product, reduce the consumption of manpower, further improve washing, the separation efficiency of polyphenylene sulfide particle.
3) adopt stainless steel sintering filter plate as separate the medium of different grain size particle in solution, not only can bear higher material pressure, and corrosion-resistant, be applicable to industrialized unit.
4) outside of washing cavities and collecting chamber is adopted and is welded to connect, and when can avoid encrypting the seal connection with flange, causes the problem of leakage after material or washing composition dissolve the sealing-ring burn into.
5) adopt lifting device to take out the good material of washing in conjunction with turning device; the more situation of charging capacity in the time of also can adapting to the mass-producing washing; not only reduce the consumption of manpower, and solved the problem that the solid materials in darker greatly still is difficult to shift away.
Description of drawings
Fig. 1 is the washing machine structure schematic diagram that a kind of method that improves the washing of polyphenylene sulfide particle, separation efficiency of the present invention is used.
In figure:
The 1-condenser, 2-condensed fluid collection tank, 3-liquidometer, 4-whipping appts, 5-charging opening, the 6-kettle cover, 7-washing cavities, 8-heating jacket, 9-kettle lifting screens, 10-stainless steel sintering filter plate, 11-puts circle, 12-collecting chamber, 13-bleed valve, 14-turning device, 15-screw block.
Embodiment
Embodiment
In polyphenylene sulfide synthetic, product can not reach uniform molecular weight, and the granularity of the polymkeric substance that obtains is also just different, but the particle diameter of the polyphenylene sulfide particle more than 95% is more than 75 μ m, and the polyphenylene sulfide particle of remainder is just less than 75 μ m.Also can the sodium chloride particle of by-product polyphenylene sulfide total mass more than 1 times in building-up process.The granularity of sodium-chlor is all less than 20 μ m, and sodium-chlor can be water-soluble, can remove by the way of washing.
Certain batch of crude product that is synthesized is carried out preliminary solid-liquid separation with vibratory screening apparatus.Because polyphenylene sulfide and by product mix, so be the particulate matter of viscous.Such polyphenylene sulfide particle is divided into several increments originally.
To the first increment originally, adopt washing machine structure as shown in Figure 1, comprise the kettle that washing cavities setting up and down 7 and collecting chamber 12 consists of, washing cavities 7 and collecting chamber 12 are separated by stainless steel sintering filter plate 10, and stainless steel sintering filter plate 10 is arranged in washing cavities 7 bottoms by putting circle 11; The agitator of whipping appts 4 stretches in the washing cavities 7 of kettle, and heating jacket 8 is positioned at washing cavities 7 peripheries, and the washing cavities bottom arranges bleed valve 13, and washing cavities 7 tops arrange the kettle cover 6 of sealing, and the condensation reflux unit of charging opening 5 and washing composition is set on kettle cover 6.Whole kettle is arranged on lifting support, and the kettle lifting screens 9 spacing to kettle is set on lifting support, and kettle drives lifting by screw block 15, is overturn by turning device 14, topples over material wherein.The joint that is communicated with condenser 1 tube side import is set, the condensed fluid collection tank 2 of the tube side outlet tape splicing liquidometer 3 of condenser 1 on kettle cover.
Concrete washing step is:
First increment that a) will wash originally is placed in the washing cavities of washing machine;
B) first add acetone as washing composition, cover the first increment basis that to wash;
C) washing composition is heated as heating medium with the hot water of 50 ± 2 ℃, adopt 200 purpose stainless steel sintering filter plates; Whipping appts by washing machine stirs the first increment originally and washing composition fully, makes the particle separation of different-grain diameter; Less than the molecule (particle diameter is less than 75 μ m) in the corresponding aperture of 200 purpose stainless steel sintering filter plates, greater than washing composition density, pass stainless steel sintering filter plate from washing cavities because of its density in the particle of separating, isolated in time, collect in collecting chamber;
D) after washing finishes, stops stirring 10 minutes, open bleed valve, emit and contain particle diameter less than the washing composition of the molecule of 75 μ m, the polyphenylene sulfide particle that wash is stayed in washing cavities, then turns off bleed valve;
E) adopt successively respectively tap water, tap water to add washing cavities as washing composition, repeat above-mentioned steps c)～d), in order to dissolve, wash away the sodium chloride particle of by-product;
F) adopting successively respectively mass concentration is 0.3% acetic acid solution, distilled water and distilled water, repeats above-mentioned steps c)～d) complete to washing;
G) kettle and kettle cover are separated, adopt the lifting device of washing machine that kettle is lowered, then with turning device, the good polyphenylene sulfide particle of washing is taken out in 135 ° of washing kettle upsets, the polyphenylene sulfide particle is placed in dryer, oven dry is 8 hours at the temperature of 110 ± 2 ℃, after cool to room temperature, obtain the larger polyphenylene sulfide particle of granularity in loft drier.
Then, measure its melt mass flow rate with the melt flow rate (MFR) determinator under 315 ℃, the condition in 5kg load, 2.095mm mouth nib footpath, be 162g/10min, meet that company standard requires≤requirement of 180 g/10min.
to the second increment originally, place it in common filter plate or the filter screen of not containing, do not have collecting chamber but below also have in the container of bleed valve, first use acetone as washing composition, with the hot water of 50 ± 2 ℃ as heating medium, opening under the condition of stirring washing one time, finish with washing with acetone, after stopping stirring 10 minutes, open the bleed valve of container bottom, material and acetone are put on the filtration unit that is provided with 200 order filter plates together, the bleed valve of turning off washing container, the material that filters out liquid is poured in this container again, after adding tap water from charging opening, wash twice, dissolve the sodium chloride particle of by-product, then be 0.3% acetic acid solution washing one time with mass concentration, then use again twice of distilled water wash, after completing the washing of said procedure, can see and still contain many molecules in the product on filtering device filter screen, the polyphenylene sulfide of this particle inequality is poured out, be placed in dryer, oven dry is 8 hours at the temperature of 110 ± 2 ℃, be cooled to room temperature in loft drier after, obtain the polyphenylene sulfide particle of granularity inequality.
Measure its melt mass flow rate with the melt flow rate (MFR) determinator under 315 ℃, the condition in 5kg load, 2.095mm mouth nib footpath, be 1350g/10min, do not reach far that company standard requires≤requirement of 180 g/10min.
to the 3rd increment originally, place it in common filter plate or the filter screen of not containing, do not have collecting chamber but below also have in the container of bleed valve, with acetone as washing composition, with the hot water of 50 ± 2 ℃ as heating medium, opening under the condition of stirring washing one time, finish with washing with acetone, after stopping stirring 10 minutes, open the bleed valve of container bottom, material and acetone are put on the filtration unit that is provided with 200 order filter plates together, the bleed valve of turning off washing container, again pour the material that filters out liquid into this container, add acetone from charging opening, wash again twice with acetone, again with washing from the beginning twice, dissolve the sodium chloride particle of by-product, then be 0.3% acetic acid solution washing one time with mass concentration, then use again twice of distilled water wash, after completing the washing of said procedure, can see and still be mingled with a small amount of molecule in the product on filtering device filter screen, this polyphenylene sulfide is poured out, be placed in dryer, oven dry is 8 hours at the temperature of 110 ± 2 ℃, be cooled to room temperature in loft drier after, obtain still being mingled with the polyphenylene sulfide of a small amount of molecule.
Measure its melt mass flow rate with the melt flow rate (MFR) determinator under 315 ℃, the condition in 5kg load, 2.095mm mouth nib footpath, be 206g/10min, do not reach still that company standard requires≤requirement of 180 g/10min.
Contrast the detected result of the product that obtains after the different washing methods of above-mentioned three these processes of increment, can find to adopt a kind of method that adopts special washing machine to improve the washing of polyphenylene sulfide particle, separation efficiency provided by the invention, can effectively improve washing, the separation efficiency of p-poly-phenyl thioether particle, save the consumption of washing composition, reduce material from the product loss of carrying and the consumption of manpower back and forth between washing container and filtration unit.
Claims (2)
1. method that improves polyphenylene sulfide particle washing, separation efficiency, be mainly and adopt the washing machine that is separated into washing cavities and collecting chamber and has a whipping appts by stainless steel sintering filter plate to wash, the collecting chamber bottom arranges bleed valve, the washing cavities top arranges the kettle cover of sealing, the condensation reflux unit of charging opening and washing composition is set on kettle cover, it is characterized in that described method mainly comprises the following steps:
The polyphenylene sulfide particle that will wash is placed in the washing cavities of washing machine;
First add acetone as washing composition, cover the polyphenylene sulfide particle that will wash;
Hot water with 48～55 ℃ heats washing composition as heating medium, adopts the stainless steel sintering filter plate of setting the order number; Whipping appts by washing machine stirs polyphenylene sulfide particle and the washing composition that will wash fully, makes the particle separation of different-grain diameter; In the particle of separating less than set molecule that order counts stainless steel sintering filter plate corresponding aperture because of density greater than washing composition density, pass stainless steel sintering filter plate from washing cavities, isolated in time, collected in collecting chamber;
Washing finishes, and after stopping stirring 10 minutes, opens bleed valve, emits the washing composition that contains molecule, and the polyphenylene sulfide particle that wash is stayed in washing cavities, then closes bleed valve;
Adopt successively respectively tap water, tap water to add washing cavities as washing composition, repeat above-mentioned steps c)～d), in order to dissolve, wash away the sodium chloride particle of by-product;
Adopting successively respectively mass concentration is that 0.1%～0.5% acetic acid solution, distilled water and distilled water add washing cavities as washing composition, repeats above-mentioned steps c)～d) complete to washing;
Kettle and kettle cover are separated, adopt the lifting device of washing machine to take out the good polyphenylene sulfide particle of washing in conjunction with turning device, the polyphenylene sulfide particle is placed in dryer, oven dry is 8 hours at the temperature of 110 ± 5 ℃, after cool to room temperature, obtain the larger polyphenylene sulfide particle of granularity in loft drier.
2. the method for raising polyphenylene sulfide particle according to claim 1 washing, separation efficiency is characterized in that: the washing cavities of described washing machine and the housing of collecting chamber adopt and are welded to connect.
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| CN201310117405.9A CN103172863B (en) | 2013-04-07 | 2013-04-07 | Method for improving washing and separating efficiency of polyphenylene sulfide particles |
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| CN201310117405.9A CN103172863B (en) | 2013-04-07 | 2013-04-07 | Method for improving washing and separating efficiency of polyphenylene sulfide particles |
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| CN103172863B CN103172863B (en) | 2015-02-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219135A (en) * | 2017-12-25 | 2018-06-29 | 浙江新和成特种材料有限公司 | A kind of continuous washing device of polyphenylene sulfide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219135A (en) * | 2017-12-25 | 2018-06-29 | 浙江新和成特种材料有限公司 | A kind of continuous washing device of polyphenylene sulfide |
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| CN103172863B (en) | 2015-02-25 |
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Address after: 226200 Changjiang Town, Rugao City, Rugao, Nantong, Jiangsu, No. 6, Xiangjiang Road Co-patentee after: Jiangsu hundred Sichuan high science and technology new materials Limited by Share Ltd Patentee after: Nantong hundred Sichuan new materials Co., Ltd. Address before: 226500 Rugao, Jiangsu City, the Yangtze River town (Rugao port) Shannon Road, No. 6 Co-patentee before: Wuxi Baichuan Chemical Industrial Co., Ltd. Patentee before: Baichuan Chemical (Rugao) Co., Ltd. |
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