CN103172863B - 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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- CN103172863B CN103172863B CN201310117405.9A CN201310117405A CN103172863B CN 103172863 B CN103172863 B CN 103172863B CN 201310117405 A CN201310117405 A CN 201310117405A CN 103172863 B CN103172863 B CN 103172863B
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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 improving the washing of polyphenylene sulfide particle, separation efficiency.
Background technology
In general for the solid particulate of drying, by sieving, varigrained particulate matter can be separated, can by filtering solid filtering out for the solid in liquid phase.But when there is the particulate matter of different-grain diameter in solution, or when surface particles humidity, viscous, when the particulate matter of small (being less than certain setting particle diameter) is adsorbed on large surface particles, the particulate matter of different-grain diameter be allowed separately just to seem more difficult.
Traditional method adopts suitable solvent or medium, under the condition stirred, the molecule of surface particles absorption is temporarily separated, but when stirring one stop, preparing filter time, again can be precipitated again by the molecule be temporarily separated, be adsorbed on oarse-grained surface, cause the poor effect of washing, being separated, need, by repeatedly washing, constantly diluting, corresponding effect could be obtained, this adds increased the number of times of washing, add the consumption of washing composition.
At synthetic macromolecular compound, such as during polyphenylene sulfide, polymer substance, because of the difference of chaining length, can form the particulate matter of different-grain diameter.Along with the difference of particle size, the performance of their physics, chemistry also can be caused different, in order to make the performance of the product obtained convergent as far as possible, need to wash product with washing composition etc., and wish while washing, in passing the particulate matter of different-grain diameter separately, after washing is over, can also easily the particulate matter of having washed can also be taken out.
The english abbreviation of polyphenylene sulfide is PPS, is a kind of high performance thermoplastic resin, the advantage such as have that physical strength is high, high temperature resistant, chemical resistance corrosion, difficult combustion, Heat stability is good, electrical property are excellent.All be widely used at electronics, automobile, machinery and chemical field.
The deficiency existed for existing conventional washing apparatus and the actual requirement to particulate matter washing effect, consider to research and develop a kind of particulate matter, particularly polyphenylene sulfide particle of improving, 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 improving the washing of polyphenylene sulfide particle, separation efficiency, when washing the polyphenylene sulfide particle of different-grain diameter, not only the liquid of the viscous of polyphenylene sulfide particle surface absorption can be washed off, and the molecule that large particle surface adheres to can be separated in time, improve the washing of polyphenylene sulfide particle, separation efficiency, and avoid possible loss in object 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 improving the washing of polyphenylene sulfide particle, separation efficiency, be mainly to adopt and sinter filter plate by stainless steel and be separated into washing cavities and collecting chamber and the washing machine with whipping appts washs, bottom collecting chamber, bleed valve is set, washing cavities top arranges the kettle cover of sealing, kettle cover is arranged the condensation reflux unit of charging opening and washing composition, 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) as heating medium, washing composition is heated with the hot water of 48 ~ 55 DEG C, adopt the stainless steel sintering filter plate of setting order number; Stirred the polyphenylene sulfide particle and washing composition that will wash by the whipping appts of washing machine fully, make the particle separation of different-grain diameter; The molecule being less than the corresponding aperture of setting order number stainless steel sintering filter plate in the particle separated is greater than washing composition density because of density, from washing cavities through stainless steel sintering filter plate, is isolated in time, collects in collecting chamber;
D) washing terminates, and stop stirring after 10 minutes, open bleed valve, release the washing composition containing molecule, the polyphenylene sulfide particle that wash is stayed in washing cavities, then closes bleed valve;
E) adopt tap water successively respectively, tap water add washing cavities as washing composition, repeat above-mentioned steps c) ~ d), to dissolve, to wash away the sodium chloride particle of by-product;
F) adopt successively respectively mass concentration be 0.1% ~ 0.5% acetic acid solution, distilled water and distilled water add washing cavities as washing composition, repeat above-mentioned steps c) ~ d) to having washed;
G) kettle and kettle cover are separated, the lifting device of washing machine is adopted to take out the polyphenylene sulfide particle washed in conjunction with turning device, polyphenylene sulfide particle is placed in dryer, dry 8 hours at the temperature of 110 ± 5 DEG C, in loft drier after cool to room temperature, obtain the polyphenylene sulfide particle that granularity is larger.
Further, the washing cavities of described washing machine and the housing of collecting chamber adopt and are welded to connect.
The invention has the advantages that:
1) separate with stainless steel sintering filter plate between washing cavities and collecting chamber, passed stainless steel sintering filter plate by the molecule that washing composition is temporarily separated because density is comparatively large when making to wash, be collected in collecting chamber in time.Owing to there is no agitating vane in collecting chamber, liquid wherein do not have the washing composition in washing cavities to move so severe, these sediments are just not easy to rise again, cover separate molecule polyphenylene sulfide macrobead (object product) on, the washing of polyphenylene sulfide particle, separation efficiency can be improved.
2) when certain washing terminates, when opening the bleed valve of collecting chamber bottom, molecule can be discharged together in company with washing composition, after closing bleed valve, the polyphenylene sulfide particle that will wash need not be taken out, add the washing that fresh washing composition just can start next time, thus not only can avoid the possible loss in transfer process of object product, reduce the consumption of manpower, improve the washing of polyphenylene sulfide particle, separation efficiency further.
3) adopt stainless steel sintering filter plate as the medium being separated different grain size particle in the solution, not only can bear higher material pressure, and corrosion-resistant, be applicable to industrialized unit.
4) outside of washing cavities and collecting chamber adopts and is welded to connect, and when can avoid connecting with flange encryption seal, causes the problem of leakage after material or washing composition dissolve sealing-ring burn into.
5) lifting device is adopted to take out the material washed in conjunction with turning device; also the situation that when mass-producing is washed, charging capacity is more can be adapted to; not only reduce the consumption of manpower, and the solid materials solved in comparatively large darker still is difficult to the problem that shifts away.
Accompanying drawing explanation
Fig. 1 be the present invention a kind of improve polyphenylene sulfide particle washing, separation efficiency method use washing machine structure schematic diagram.
In figure:
1-condenser, 2-condensed fluid collection tank, 3-liquidometer, 4-whipping appts, 5-charging opening, 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 the synthesis of polyphenylene sulfide, product can not reach uniform molecular weight, and the granularity of the polymkeric substance obtained is also just different, but the particle diameter of the polyphenylene sulfide particle of more than 95% is more than 75 μm, and the polyphenylene sulfide particle of remainder is just less than 75 μm.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 μm, and sodium-chlor can be water-soluble, can be removed by the way of washing.
The crude product vibratory screening apparatus be synthesized certain batch carries out preliminary solid-liquid separation.Because polyphenylene sulfide and by product mix, so be the particulate matter of viscous.Such polyphenylene sulfide particle is divided into several increment originally.
To the first increment originally, adopt washing machine structure as shown in Figure 1, comprise the kettle of washing cavities 7 setting up and down and collecting chamber 12 formation, washing cavities 7 and collecting chamber 12 sinter filter plate 10 by stainless steel and separate, and stainless steel sintering filter plate 10 is arranged in washing cavities 7 bottom by putting circle 11; The agitator of whipping appts 4 stretches in the washing cavities 7 of kettle, and it is peripheral that heating jacket 8 is positioned at washing cavities 7, arranges bleed valve 13 bottom washing cavities, and washing cavities 7 top arranges the kettle cover 6 of sealing, kettle cover 6 is arranged the condensation reflux unit of charging opening 5 and washing composition.Whole kettle is arranged on lifting support, and lifting support is arranged the kettle lifting screens 9 spacing to kettle, kettle drives lifting by screw block 15, is overturn by turning device 14, topples over material wherein.Kettle cover is arranged the joint being communicated with the import of condenser 1 tube side, the condensed fluid collection tank 2 of the tube side outlet tape splicing liquidometer 3 of condenser 1.
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 will wash;
C) as heating medium, washing composition is heated with the hot water of 50 ± 2 DEG C, adopt 200 object stainless steel sintering filter plates; Stir the first increment basis and washing composition fully by the whipping appts of washing machine, make the particle separation of different-grain diameter; Be less than the molecule (particle diameter is less than 75 μm) in the 200 corresponding apertures of object stainless steel sintering filter plate in the particle separated, because its density is greater than washing composition density, from washing cavities through stainless steel sintering filter plate, isolated in time, collect in collecting chamber;
D) washing terminates, stops stirring after 10 minutes, and open bleed valve, release the washing composition being less than the molecule of 75 μm containing particle diameter, the polyphenylene sulfide particle that wash is stayed in washing cavities, then turns off bleed valve;
E) adopt tap water successively respectively, tap water add washing cavities as washing composition, repeat above-mentioned steps c) ~ d), to dissolve, to wash away the sodium chloride particle of by-product;
F) adopt successively respectively mass concentration be 0.3% acetic acid solution, distilled water and distilled water, repeat above-mentioned steps c) ~ d) to having washed;
G) kettle and kettle cover are separated, adopt the lifting device of washing machine that kettle is lowered, then with turning device, washing kettle is overturn 135 ° to take out the polyphenylene sulfide particle washed, polyphenylene sulfide particle is placed in dryer, dry 8 hours at the temperature of 110 ± 2 DEG C, in loft drier after cool to room temperature, obtain the polyphenylene sulfide particle that granularity is larger.
Then, with melt flow rate (MFR) determinator 315 DEG C, 5kg load, 2.095mm mouth nib footpath condition under measure its melt mass flow rate, be 162g/10min, meet that company standard requires≤requirement of 180 g/10min.
To the second increment originally, place it in common not containing filter plate or filter screen, there is no collecting chamber but have in the container of bleed valve below yet, first use acetone as washing composition, with the hot water of 50 ± 2 DEG C as heating medium, wash one time under the condition opening stirring, terminate with washing with acetone, stop stirring after 10 minutes, open the bleed valve of lower vessel portion, material is put into together with acetone be provided with 200 order filter plates filtration unit on, turn off the bleed valve of washing container, the material filtering 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 one time is washed with the acetic acid solution that mass concentration is 0.3%, then distilled water wash twice is used again, after completing the washing of said procedure, can see in the product on filtering device filter screen still containing many molecules, the polyphenylene sulfide of this particle inequality is poured out, be placed in dryer, dry 8 hours at the temperature of 110 ± 2 DEG C, be cooled to room temperature in loft drier after, obtain the polyphenylene sulfide particle of granularity inequality.
With melt flow rate (MFR) determinator 315 DEG C, 5kg load, 2.095mm mouth nib footpath condition under measure its melt mass flow rate, be 1350g/10min, far do not reach that company standard requires≤requirement of 180 g/10min.
To the 3rd increment originally, place it in common not containing filter plate or filter screen, there is no collecting chamber but have in the container of bleed valve below yet, with acetone as washing composition, with the hot water of 50 ± 2 DEG C as heating medium, wash one time under the condition opening stirring, terminate with washing with acetone, stop stirring after 10 minutes, open the bleed valve of lower vessel portion, material is put into together with acetone be provided with 200 order filter plates filtration unit on, turn off the bleed valve of washing container, again the material filtering out liquid is poured into this container, acetone is added from charging opening, twice is washed again with acetone, again with washing twice from the beginning, dissolve the sodium chloride particle of by-product, then one time is washed with the acetic acid solution that mass concentration is 0.3%, then distilled water wash twice is used again, after completing the washing of said procedure, can see in the product on filtering device filter screen and still be mingled with a small amount of molecule, this polyphenylene sulfide is poured out, be placed in dryer, dry 8 hours at the temperature of 110 ± 2 DEG C, be cooled to room temperature in loft drier after, still be mingled with the polyphenylene sulfide of a small amount of molecule.
With melt flow rate (MFR) determinator 315 DEG C, 5kg load, 2.095mm mouth nib footpath condition under measure its melt mass flow rate, be 206g/10min, still do not reach that company standard requires≤requirement of 180 g/10min.
Contrast the detected result of this product obtained after different washing methodss of above-mentioned three increments, can find adopt provided by the invention a kind of adopt special washing machine to improve polyphenylene sulfide particle washing, separation efficiency method, effectively can improve washing, the separation efficiency of p-poly-phenyl thioether particle, save the consumption of washing composition, reduce the consumption of material from the product loss carried back and forth between washing container and filtration unit and manpower.
Claims (2)
1. one kind is improved the method for the washing of polyphenylene sulfide particle, separation efficiency, be mainly to adopt and sinter filter plate by stainless steel and be separated into washing cavities and collecting chamber and the washing machine with whipping appts washs, bottom collecting chamber, bleed valve is set, washing cavities top arranges the kettle cover of sealing, kettle cover is arranged the condensation reflux unit of charging opening and washing composition, it is characterized in 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) as heating medium, washing composition is heated with the hot water of 48 ~ 55 DEG C, adopt the stainless steel sintering filter plate of setting order number; Stirred the polyphenylene sulfide particle and washing composition that will wash by the whipping appts of washing machine fully, make the particle separation of different-grain diameter; The molecule being less than the corresponding aperture of setting order number stainless steel sintering filter plate in the particle separated is greater than washing composition density because of density, from washing cavities through stainless steel sintering filter plate, is isolated in time, collects in collecting chamber;
D) washing terminates, and stop stirring after 10 minutes, open bleed valve, release the washing composition containing molecule, the polyphenylene sulfide particle that wash is stayed in washing cavities, then closes bleed valve;
E) adopt tap water successively respectively, tap water add washing cavities as washing composition, repeat above-mentioned steps c) ~ d), to dissolve, to wash away the sodium chloride particle of by-product;
F) adopt successively respectively mass concentration be 0.1% ~ 0.5% acetic acid solution, distilled water and distilled water add washing cavities as washing composition, repeat above-mentioned steps c) ~ d) to having washed;
G) kettle and kettle cover are separated, the lifting device of washing machine is adopted to take out the polyphenylene sulfide particle washed in conjunction with turning device, polyphenylene sulfide particle is placed in dryer, dry 8 hours at the temperature of 110 ± 5 DEG C, in loft drier after cool to room temperature, obtain the polyphenylene sulfide particle that granularity is larger.
2. the method for raising polyphenylene sulfide particle washing according to claim 1, separation efficiency, is characterized in that: the washing cavities of described washing machine and the housing of collecting chamber adopt and be 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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| CN103172863B true CN103172863B (en) | 2015-02-25 |
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| CN108219135B (en) * | 2017-12-25 | 2021-05-04 | 浙江新和成特种材料有限公司 | Continuous washing device of polyphenylene sulfide resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4507468A (en) * | 1982-07-16 | 1985-03-26 | Dainippon Ink And Chemicals, Inc. | Method for purifying polyphenylene sulfide |
| JPH0643490B2 (en) * | 1986-03-24 | 1994-06-08 | 東都化成株式会社 | Purification method of polyphenylene sulfide |
| JPS62263224A (en) * | 1986-05-12 | 1987-11-16 | Toray Ind Inc | Production of polyphenylene sulfide |
| CA2101409A1 (en) * | 1992-10-23 | 1994-04-24 | Earl Clark Jr. | Production of poly(arylene sulfide) polymers containing reduced amounts of oligomers |
| JP2007262341A (en) * | 2006-03-30 | 2007-10-11 | Toray Ind Inc | Purification method of polyarylene sulfide resin |
| CN101429280A (en) * | 2008-12-09 | 2009-05-13 | 江苏新中投资有限公司 | Continuous washing method for product in polyphenylene sulfide production |
| EP2572779A4 (en) * | 2010-05-21 | 2016-09-07 | Kureha Corp | Vertical countercurrent solid-liquid contact method, method for washing solid particles, method for producing polyarylene sulfide, and device therefor |
| JP5805084B2 (en) * | 2010-07-13 | 2015-11-04 | 株式会社クレハ | Method and apparatus for producing polyarylene sulfide |
| CN102675641B (en) * | 2011-03-18 | 2014-04-02 | 四川得阳工程塑料开发有限公司 | Product purification treatment process for polyphenylene sulfide production |
| CN102731785B (en) * | 2012-06-11 | 2014-04-09 | 张家港市新盛新材料有限公司 | Polyphenylene sulfide purifying method |
| CN102863622A (en) * | 2012-09-25 | 2013-01-09 | 自贡鸿鹤化工股份有限公司 | Method for collecting polyphenylene sulfide resin from polyphenylene sulfide resin slurry |
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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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