CN102585206B - Polyether ketone refining process - Google Patents
Polyether ketone refining process Download PDFInfo
- Publication number
- CN102585206B CN102585206B CN 201210057660 CN201210057660A CN102585206B CN 102585206 B CN102585206 B CN 102585206B CN 201210057660 CN201210057660 CN 201210057660 CN 201210057660 A CN201210057660 A CN 201210057660A CN 102585206 B CN102585206 B CN 102585206B
- Authority
- CN
- China
- Prior art keywords
- acetone
- water
- refining kettle
- valve
- steam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention discloses a novel polyether ketone refining process, belonging to the fields of chemical engineering and fine chemistry industry, and particularly relates to a process for refinishing polyether ketone. A technical process comprises the following steps of: I, extensively leaching acetone repeatedly, and quickly feeding all diphenyl sulfone in polyether ketone in a refining kettle into an acetone solution of an acetone evaporation kettle to realize separation of diphenyl sulfone from polyether ketone; II, washing with water; III, drying; and IV, extracting a material, and cleaning the material in an air purging state. The process has the advantages of centralized equipment, small floor area, small overall investment, short production period, high efficiency, small quantity of operating personnel, convenience for managing, high production benefit, saving in energy consumption, zero discharge of pollutants in a production process, realization of high diphenyl sulfone leaching efficiency, low boiling point of acetone, small storage amount of an acetone tank and reduction in the energy consumption in the extensive leaching process of an acetone liquid, and capability of greatly saving energy since the waste water handling capacity is low in a water washing process, and is a novel environmentally-friendly chemical process.
Description
Technical field
The invention belongs to chemical engineering, field of fine chemical, particularly relate to the technique of refining a kind of polyetherketone.
Background technology
Polyetherketone of the prior art be the earliest Britain ICI company with sulfobenzide as solvent, 4,4-difluoro benzophenone and Resorcinol be as raw material, synthetic through the nucleophilic substitution condensation reaction in the situation that salt of wormwood or yellow soda ash exist.In succession develop multiple series polyethers ketone high polymeric compound over past ten years.The common feature of reaction product is: after reaction finished, product, solvent, by product etc. were entrained in together, form solid mixture under the normal temperature.Principal reaction thing 4,4-difluoro benzophenone and Resorcinol all participate in reaction in the product.Usually blended solid is pulverized, the sulfobenzide solvent when leaching polyreaction with organic solvent, water leaches by product villiaumite and raw material salt of wormwood etc. again, and then drying obtains pure polyetherketone.This process often is called again polyether ketone refinement.
When sulfobenzide leached, document and current technology adopted following several techniques.Fig. 2 is extraction process, and Fig. 3 is fat extraction technique, and Fig. 4 is circulation technology, and Fig. 5 is digesting technoloy, and Fig. 6 is the liquid flooding extraction process.
Extraction process: the polyetherketone material pneumatic that will contain sulfobenzide is transported among the reactor R1, in time from storage tank C to reactor R1 pumping acetone.Open the heating of reactor R1 steam inlet valve, temperature is controlled at 40 ℃.Open reactor R1 bottom discharge valve, regulate the flow that pumps into acetone, the liquid level in the control reactor R1.After reactor R1 effluent enters reactor R2, after liquid level reach a certain height among the question response still R2, logical steam, heating, distillation in the reactor R2, the acetone of outflow is directly put into reactor R1, and the liquid level of keeping two stills is at certain altitude.When sulfobenzide concentration reaches processing requirements in the reactor R1 solution, reactor R1 stopped heating, and liquid whole reactor R2 that put in batches that will be wherein distill, distillate is put into storage tank C.When solution among the reactor R2 when saturated, solution is put in the moisture eliminator dry, reclaims sulfobenzide.This technique outstanding problem is that energy consumption is higher.
Fat extraction formula technique: the polyetherketone material pneumatic that will contain sulfobenzide is transported among the reactor R1, from storage tank to leaching pumping acetone the still R1, makes acetone soln just flood material in the still.After about 5 minutes, open reactor R1 bottom tap valve and still top compressed air regulating valve, acetone soln among the reactor R1 all is pressed among the reactor R2 off-response still R1 baiting valve and compressed air regulating valve, open the blow-off valve of reactor R1, make among the reactor R1 Pressure Drop to normal pressure.Pass into steam heating in the chuck of reactor R2, wherein the steam that flows out of distillation enters the condenser on reactor R1 top, phlegma flows back in the reactor R1.When sulfobenzide among the reactor R2 when saturated, the solution in the reactor R2 is put into moisture eliminator, obtain the solvent sulfobenzide through the scraping blade drying.Liquid level causes liquid measure inadequate because part acetone solution is released in the reactor R1, can do suitably to replenish in reactor R1.Acetone soln kept in reactor R1 5 minutes again, open the top compressed air regulating valve of tap valve at the bottom of the reactor R1 still, reactor R1, acetone soln among the reactor R1 all is pressed among the reactor R2, repeat above operation, until the sulfobenzide content of acetone soln reaches requirement among the reactor R1.
Circulation technology: the polyetherketone material pneumatic that will contain sulfobenzide is transported among the reactor R1, in time from storage tank A to reactor R1 pumping acetone, and in time start reactor R1 stirring rake, prevent the material caking.Open the heating of reactor R1 steam inlet valve, 40 ℃ of temperature controls.Open reactor R1 bottom discharge valve, regulate the acetone flow of pumping reactor R1, liquid level in the control reactor R1.After processing for some time, solution among the reactor R1 all is pressed among the reactor R2.Lead to steam, heating, distillation in reactor R2, the acetone of outflow is put into storage tank A.Note the sulfobenzide concentration of solution among the detection reaction still R2, the state that can not reach capacity prevents sulfobenzide crystallization in reactor R2.When sulfobenzide among the reactor R2 when saturated, the solution in the reactor R2 is put in the moisture eliminator, obtain sulfobenzide through the scraping blade drying.Because sulfobenzide concentration is higher in the front solution of processing several times, directly distills.Sulfobenzide concentration in the later stage leaching liquid is lower, is energy efficient, and leaching liquid is directly put into storage tank B to storage tank F tank successively without distillation, as the front several times leaching liquid of next batch material.
Digesting technoloy: the polyetherketone material pneumatic that contains sulfobenzide is transported among the reactor R, and pumps into acetone in time from the C1 storage tank to R, in time start the R stirring rake.Open the heating of R steam inlet valve, temperature is controlled in 40 ℃. the always boiling of later time, until after sulfobenzide reached higher concentration in the solution in the still, then the disposable interior solution of still of all emitting, pumped into the fresh acetone leaching again.Through repeatedly repeating leaching, until sulfobenzide content reaches production requirement in the solution.
Liquid flooding extraction process: the polyetherketone material pneumatic that contains sulfobenzide is transported among the reactor R1, to acetone evaporated still R2, pumps into acetone from storage tank, simultaneously, open reactor R1 bottom valve and top thereof the variable valve of giving vent to anger.Heating acetone evaporated still R2, the acetone steam in the acetone evaporated still R2 enters among the reactor R1, passes through the material back up pad and contacts with polyetherketone, finishes mass transfer, heat transfer process.The acetone steam of partial condensation rests among the reactor R1, and all the other acetone steams enter the interchanger condensation by the material of reactor R1, and phlegma flows among the reactor R1 again.After the acetone liquid level of having dissolved a certain amount of sulfobenzide among the reactor R1 reach a certain height, open reactor R1 bottom valve, acetone among the reactor R1 flows among the acetone evaporated still R2 by gravity, simultaneously, open acetone evaporated still R2 by-pass valve, acetone steam directly enters the interchanger condensation, and phlegma flows among the reactor R1 again.So repeat, the sulfobenzide among the reactor R1 in the polyetherketone enters in the acetone soln of acetone evaporated still R2, until the sulfobenzide content of acetone soln reaches requirement among the reactor R1.
Circulation technology needs to arrange eight above acetone mixed solution storage tanks because the leaching number of times is more in the technique.And energy consumption is higher relatively.Digesting technoloy process and circulation technology approach, but because mass transfer factor, this process efficiency will be lower than circulation technology.Extraction process relies on Matter Transfer in the system, saves time, and process is simple, and the acetone consumption is few, but shortcoming is the energy consumption height.Fat extraction, and liquid flooding (improvement fat extraction) formula technique relatively effective, but leaching still structure is special, the problems such as line clogging also occur once in a while.
Water extraction: the water extraction process is commonly referred to washing.A kind of technique is exactly at a slow speed, use poach under the intermittent stirring, boils to a certain degree water is emitted, and then adds fresh water, until the water-soluble substanceses such as villiaumite are cleaned.Another kind of technique is to consider that stirring can make the material efflorescence, the form that adopts recirculated water to flow is strengthened mass transfer process, namely adds water outlet washing the still bottom, adds simultaneously filtration unit, the inner upper end of reactor is provided with water inlet distribution pipe, and water is squeezed into the bottom and flowed out and to loop from washing still top through recycle pump.
Dry: leach sulfobenzide, wash out after the villiaumite etc. through acetone, the polyetherketone product is removed through centrifugation and is wherein soaked the most of moisture that contains, and enters drying process.The granule materials dried forms is more, can adopt the single cell operating equipment, also can adopt Combined drying equipment.The vacuum-drying of present most process using double cone dryer obtains pure material at last.The drying of this kind form because temperature is higher in the system, is rich in water vapour, and when lowering the temperature blowing, moisture comes back to the material surface, during detection the moisture increase larger, reach drying and require consuming time longer.
Fluoride waste is processed: produce waste water containing fluorine in water washing process, the quality that generally produces waste water is 10～15 times of polyetherketone treatment capacity.Adopt distillating method can reclaim villiaumite, also can utilize the water that steams, but because the large energy consumption of wastewater flow rate is very big.Adopt chemical precipitation, flocculation sediment and adsorption treatment, though fluorine content can reach below the 10mg/L in the water, satisfy emission request, reduce energy consumption and processing cost, but discharging long-time, waste water containing fluorine still can cause certain pollution to environment, groundwater resource.
Above polyether ketone refinement process, every kind of technique, all there are some problems in each process.Most importantly complex technical process.Each process need multiple devices, and each process is separate, the device fabrication expense is high, and floor space is large.An operating process also needs to be connected with another process in the production, and is consuming time more in the material transfer process, affects production schedule.Operation, packing etc. have again particular requirement before and after in the simultaneously actual production, such as product particle shape, geometrical dimension etc., do not allow to occur larger variation in leaching process.Each material handling has some amount, requires as far as possible low rate mixing or does not stir, in case the material efflorescence.Whole treating process energy consumption is high, has the hidden danger of environmental pollution etc.
Summary of the invention
In order effectively to solve the deficiencies in the prior art, according to previous experiments data and the operation result, the present invention has designed a kind of more efficient, environmental protection, energy-conservation green production process.Its technological process as shown in Figure 1.Carry through vacuum material, will treat that refining polyetherketone granule materials is sent into and begin in the refining kettle to make with extra care.
A kind of Novel polyether ketone refining process is characterized in that may further comprise the steps:
Step 1 acetone liquid flooding leaching process, acetone in the acetone storage tank is sent in the acetone evaporated still through the V102 valve with the acetone transferpump, under steam-heated effect, acetone steam in the acetone evaporated still along the acetone steam pipeline in acetone steam admission port enters bottom gas distribution tube in the refining kettle, distribution through gas distribution tube, acetone steam passes through the material back up pad and contacts with polyetherketone, finishes mass transfer, heat transfer process; The acetone steam of partial condensation rests in the refining kettle, and all the other acetone steams enter in the interchanger by the material bed of refining kettle, and phlegma flows back in the refining kettle through surge tank, reflux pipeline again; When the acetone soln liquid level that contains sulfobenzide in the refining kettle reach the still volume 1/3 after, the V113 valve is opened automatically, acetone in the refining kettle and sulfobenzide lean on flow by gravity in the acetone evaporated still, while V109 valve autoshutdown, the V110 valve is opened automatically, acetone steam is through the interchanger condensation, and phlegma flows in the refining kettle through reflux pipeline again; Liquid sealing pipe prevents that acetone steam from entering in the refining kettle from here; Repeat above operation, the sulfobenzide in the refining kettle in the polyetherketone fast, all enters in the acetone soln of acetone evaporated still, and the realization sulfobenzide separates with polyetherketone;
The step 2 water washing process will be stored in the ultrapure water of specific conductivity in the ultrapure water storage tank≤0.1, pumps in the refining kettle by the V103 valve after being pumped by pure water pump; When the water level in the refining kettle just soaked material, close pure water pump; Pass into the steam of heating in the chuck of refining kettle, steam off when treating that water temperature is near 40 ℃ in the refining kettle; Open the V114 valve, and the water in the refining kettle all put into contain the acetone water storage tank, deliver to rectifying workshop acetone and water by containing acetone water transferpump again, reclaim wherein acetone;
Close the V114 valve, again start pure water pump, in refining kettle, add ultrapure water; When the water level in the refining kettle was higher than overflow port, the water in the refining kettle can flow automatically in the mixing water storage tank through the V116 valve; Reach three of mixing water storage tank/two o'clock in the water storage tank to be mixed, close pure water pump, in the chuck of refining kettle, pass into warmed-up steam, when treating that the interior water temperature of refining kettle reaches 80 ℃, the ON cycle pump, ultrapure water is through V120 valve, refining kettle and the circulation of mixing water storage tank; The situation that keeps recirculated water to flow; Close the V120 valve after 20 minutes, allow fluorinated water flow through membrane separation unit and electric desalination plant, by regulating the V123 valve and regulating V124 valve control aquifer yield, this water outlet is fluorinated water; Through 3 hours～5 hours circulation, treat in the refining kettle that the fluorinion concentration of the aqueous solution reaches 10ppm and when remaining unchanged, finish water washing process;
The step 3 drying process passes into the steam of heating in the chuck of refining kettle, starts simultaneously vacuum pump, through the air outlet valve place with refining kettle in air, steam take away; When the thermometer indicator value reached 100 ℃ in the refining kettle, the air of the crossing heated drying preheating of in the future auto-polymerization residual heat of reaction and that warp further heats through the filtration of F104 strainer, was sent in the refining kettle through the V101 valve again, enters the air stream drying stage; After 1 hour, detect from material conveying end feeding, when water-content in the material is mass percent≤0.02%, stop drying; Last gas drying gas gangway, and after the F103 strainer enters, flow out refining kettle;
The taking-up of step 4 material is received the material conveying end with the feeding pipe, starts the feeding vacuum pump, and opens the V127 intake valve, gets clean material under the air purge state.
When sulfobenzide concentration in the acetone soln of acetone evaporated still reaches 800ppm～1000ppm and maybe needs to reclaim wherein sulfobenzide, pass into first steam in the described step 1, the acetone that steams is all got back in the acetone storage tank by interchanger; Sulfobenzide concentration reaches capacity in the acetone soln in the acetone evaporated still, and it is emitted, and acetone, sulfobenzide are thoroughly separated.
When making water inventory reduce 1/10 owing to running off, recirculated water needs to replenish in the described step 2; The fluorinated water total amount of at every turn emitting adopts the mode of distillation to reclaim villiaumite and obtain distilled water at 1.3～1.5 tons.
Beneficial effect: adopt technique of the present invention through equipment design, manufacturing, installation and adjustment, with the Novel polyether ketone process application in production process.Equipment operation result and related data can see Table 1.
The data comparison sheet of the former technique of table 1 and novel process production run.
| Project | Former technique | Novel process |
| The refining time | 22h | 18h |
| Material water content (quality %) | 0.02% | 0.02% |
| Sulfobenzide content | ≤10ppm | ≤10ppm |
| F in the product -Concentration | ≤10ppm | ≤10ppm |
| Pulverization ratio | 2.85% | 1.68% |
| Wastewater discharge | 1.2 ton/h | 0 |
Novel process has realized the refining of polyetherketone, and its outstanding feature is: equipment is concentrated, floor space is little, whole less investment; With short production cycle, efficient is high; Operator are few, are convenient to management, improved productivity effect.The while energy efficient, the production process zero release of pollutant is a kind of novel green chemical industry technique.In acetone liquid flooding leaching process of the present invention, the sulfobenzide leaching efficiency is high, and the acetone boiling point is low, and acetone tank storage is little, reduces energy consumption.During water washing process, because wastewater treatment capacity is few, conserve energy greatly.
Description of drawings
The present invention will be further described below in conjunction with description of drawings and embodiment.
Fig. 1 is a kind of Novel polyether ketone refining process schema of the present invention.
Fig. 2 is extraction process figure in the different acetone leaching technologies of polyetherketone in the prior art.
Fig. 3 is fat extraction artwork in the different acetone leaching technologies of polyetherketone in the prior art.
Fig. 4 is circulation technology figure in the different acetone leaching technologies of polyetherketone in the prior art.
Fig. 5 is digesting technoloy figure in the different acetone leaching technologies of polyetherketone in the prior art.
Fig. 6 is liquid flooding extraction process figure in the different acetone leaching technologies of polyetherketone in the prior art.
1-acetone transferpump among the figure, the 2-V124 valve, the 3-F104 strainer, the 4-membrane separation unit, the 5-V123 valve, 6-electricity desalination plant, the 7-V120 valve, the 8-pure water pump, 9-ultrapure water storage tank, the 10-V103 valve, the 11-V102 valve, the 12-V101 valve, 13-acetone steam pipeline, 14-material conveying end, 15-material back up pad, the 16-refining kettle, the 17-V109 valve, the 18-V110 valve, the 19-F103 strainer, 20-acetone steam admission port, 21-dry gas gangway, the 22-reflux pipeline, the 23-interchanger, the 24-surge tank, the 25-overflow port, the 26-gas distribution tube, 27-contains the acetone water storage tank, the 28-liquid sealing pipe, the 29-V114 valve, the 30-V113 valve, the 31-V116 valve, 32-contains acetone water transferpump, 33-acetone evaporated still, 34-mixing water storage tank, the 35-recycle pump, the 36-V127 intake valve, 37-acetone storage tank.
Embodiment
A kind of Novel polyether ketone refining process as shown in the figure is characterized in that may further comprise the steps:
Step 1 acetone liquid flooding leaching process, acetone in the acetone storage tank 37 is sent in the acetone evaporated still 33 through V102 valve 11 with acetone transferpump 1, under steam-heated effect, acetone steam in the acetone evaporated still 33 along acetone steam pipeline 13 in acetone steam admission port 20 enters bottom gas distribution tube 26 in the refining kettle 16, distribution through gas distribution tube 26, acetone steam passes through material back up pad 15 and contacts with polyetherketone, finishes mass transfer, heat transfer process; The acetone steam of partial condensation rests in the refining kettle 16, and all the other acetone steams enter in the interchanger 23 by the material bed of refining kettle 16, and phlegma flows back in the refining kettle 16 again through surge tank 24, reflux pipeline 22; When the acetone soln liquid level that contains sulfobenzide in the refining kettle 16 reach the still volume 1/3 after, V113 valve 30 is opened automatically, acetone in the refining kettle 16 and sulfobenzide lean on flow by gravity in acetone evaporated still 33, while V109 valve 17 autoshutdowns, V110 valve 18 is opened automatically, acetone steam is through interchanger 23 condensations, and phlegma flows in the refining kettle 16 through reflux pipeline 22 again; Liquid sealing pipe 28 prevents that acetone steam from entering in the refining kettle 16 from here; Repeat above operation, the sulfobenzide in the refining kettle 16 in the polyetherketone fast, all enters in the acetone soln of acetone evaporated still 33, and the realization sulfobenzide separates with polyetherketone;
When sulfobenzide concentration in the acetone soln of acetone evaporated still 33 reaches 800ppm～1000ppm and maybe needs to reclaim wherein sulfobenzide, pass into first steam, the acetone that steams is all got back in the acetone storage tank 37 by interchanger 23; Sulfobenzide concentration reaches capacity in the acetone soln in the acetone evaporated still 33, and it is emitted, and acetone, sulfobenzide are thoroughly separated.
This technological process sulfobenzide leaching efficiency is high, and the acetone boiling point is low, and acetone tank storage is little, reduces energy consumption.
The step 2 water washing process will be stored in the ultrapure water of specific conductivity in the ultrapure water storage tank 9≤0.1, pumps in the refining kettle 16 by V103 valve 10 after being pumped by pure water pump 8; When the water level in the refining kettle 16 just soaked material, close pure water pump 8; Pass into the steam of heating in the chuck of refining kettle 16, steam off when treating that water temperature is near 40 ℃ in the refining kettle 16; Open V114 valve 29, and the water in the refining kettle 16 are all put into contain acetone water storage tank 27, deliver to rectifying workshop acetone and water by containing acetone water transferpump 32 again, reclaim wherein acetone;
Close V114 valve 29, again start pure water pump 8, in refining kettle 16, add ultrapure water; When the water level in the refining kettle 16 was higher than overflow port 25, the water in the refining kettle 16 can flow automatically in the mixing water storage tank 34 through V116 valve 31; Reach three of mixing water storage tank/two o'clock in the water storage tank 34 to be mixed, close pure water pump 8, in the chuck of refining kettle 16, pass into warmed-up steam, when treating that refining kettle 16 interior water temperatures reach 80 ℃, ON cycle pump 35, ultrapure water is through V120 valve 7, refining kettle 16 and 34 circulations of mixing water storage tank; The situation that keeps recirculated water to flow; Close V120 valve 7 after 20 minutes, allow fluorinated water flow through membrane separation unit 4 and electric desalination plant 6, by regulating V123 valve 5 and regulating V124 valve 2 control aquifer yields, this water outlet is fluorinated water; Through 3 hours～5 hours circulation, the fluorinion concentration for the treatment of the aqueous solution in the refining kettle 16 reached 10ppm and when remaining unchanged, finishes water washing process;
When making water inventory reduce 1/10 owing to running off, recirculated water needs to replenish; The fluorinated water total amount of at every turn emitting adopts the mode of distillation to reclaim villiaumite and obtain distilled water at 1.3～1.5 tons.
The step 3 drying process passes into the steam of heating in the chuck of refining kettle 16, starts simultaneously vacuum pump, through the air outlet valve place refining kettle 16 interior air, steam is taken away; When the thermometer indicator value reaches 100 ℃ in the refining kettle 16, the air of the crossing heated drying preheating of in the future auto-polymerization residual heat of reaction and that warp further heats, filter through F104 strainer 3, send in the refining kettle 16 through V101 valve 12 again, enter the air stream drying stage; After 1 hour, detect from material conveying end 14 feedings, when water-content in the material is mass percent≤0.02%, stop drying; Last gas drying gas gangway 21, and after F103 strainer 19 enters, flow out refining kettle 16;
The taking-up of step 4 material is received material conveying end 14 with the feeding pipe, starts the feeding vacuum pump, and opens V127 intake valve 36, gets clean material under the air purge state.
Claims (3)
1. polyether ketone refinement technique is characterized in that may further comprise the steps:
Step 1 acetone liquid flooding leaching process, acetone in the acetone storage tank (37) is sent in the acetone evaporated still (33) through V102 valve (11) with acetone transferpump (1), under steam-heated effect, acetone steam in the acetone evaporated still (33) is along in the bottom gas distribution tube (26) of acetone steam pipeline (13) in acetone steam admission port (20) enters refining kettle (16), distribution through gas distribution tube (26), acetone steam passes through material back up pad (15) and contacts with polyetherketone, finishes mass transfer, heat transfer process; The acetone steam of partial condensation rests in the refining kettle (16), all the other acetone steams enter in the interchanger (23) by the material bed of refining kettle (16), and phlegma flows back in the refining kettle (16) again through surge tank (24), reflux pipeline (22); When the acetone soln liquid level that contains sulfobenzide in the refining kettle (16) reach the still volume 1/3 after, V113 valve (30) is opened automatically, acetone in the refining kettle (16) and sulfobenzide arrive in the acetone evaporated still (33) by flow by gravity, while V109 valve (17) autoshutdown, V110 valve (18) is opened automatically, acetone steam is through interchanger (23) condensation, and phlegma flows in the refining kettle (16) through reflux pipeline (22) again; Liquid sealing pipe (28) prevents that acetone steam from entering in the refining kettle (16) from here; Repeat above operation, the sulfobenzide in the refining kettle (16) in the polyetherketone fast, all enters in the acetone soln of acetone evaporated still (33), and the realization sulfobenzide separates with polyetherketone;
The step 2 water washing process will be stored in the ultrapure water of specific conductivity in the ultrapure water storage tank (9)≤0.1, pump in the refining kettle (16) by V103 valve (10) after being pumped by pure water pump (8); When the water level in the refining kettle (16) just soaked material, close pure water pump (8); Pass into the steam of heating in the chuck of refining kettle (16), steam off when treating that water temperature is near 40 ℃ in the refining kettle (16); Open V114 valve (29), and the water in the refining kettle (16) all put into contain acetone water storage tank (27), deliver to rectifying workshop acetone and water by containing acetone water transferpump (32) again, reclaim wherein acetone;
Close V114 valve (29), again start pure water pump (8), in refining kettle (16), add ultrapure water; When the water level in the refining kettle (16) was higher than overflow port (25), the water in the refining kettle (16) can flow automatically in the mixing water storage tank (34) through V116 valve (31); Reach three of mixing water storage tank/two o'clock in the water storage tank to be mixed (34), close pure water pump (8), in the chuck of refining kettle (16), pass into warmed-up steam, when treating that the interior water temperature of refining kettle (16) reaches 80 ℃, ON cycle pump (35), ultrapure water is through V120 valve (7), refining kettle (16) and mixing water storage tank (34) circulation; The situation that keeps recirculated water to flow; Close V120 valve (7) after 20 minutes, allow fluorinated water flow through membrane separation unit (4) and electric desalination plant (6), by regulating V123 valve (5) and regulating V124 valve (2) control aquifer yield, this water outlet is fluorinated water; Through 3 hours～5 hours circulation, treat in the refining kettle (16) that the fluorinion concentration of the aqueous solution reaches 10ppm and when remaining unchanged, finish water washing process;
The step 3 drying process passes into the steam of heating in the chuck of refining kettle (16), starts simultaneously vacuum pump, through the air outlet valve place with refining kettle (16) in air, steam take away; When the thermometer indicator value reaches 100 ℃ in the refining kettle (16), the air of the crossing heated drying preheating of in the future auto-polymerization residual heat of reaction and that warp further heats, filter through F104 strainer (3), send in the refining kettle (16) through V101 valve (12) again, enter the air stream drying stage; After 1 hour, detect from material conveying end (14) feeding, when water-content in the material is mass percent≤0.02%, stop drying; Last gas drying gas gangway (21), and after F103 strainer (19) enters outflow refining kettle (16);
The taking-up of step 4 material is received material conveying end (14) with the feeding pipe, starts the feeding vacuum pump, and opens V127 intake valve (36), gets clean material under the air purge state.
2. a kind of polyether ketone refinement technique according to claim 1, it is characterized in that: in the described step 1 when sulfobenzide concentration in the acetone soln of acetone evaporated still (33) reaches 800ppm～1000ppm and maybe needs to reclaim wherein sulfobenzide, pass into first steam, the acetone that steams is all got back in the acetone storage tank (37) by interchanger (23); Sulfobenzide concentration reaches capacity in the acetone soln in the acetone evaporated still (33), and it is emitted, and acetone, sulfobenzide are thoroughly separated.
3. a kind of polyether ketone refinement technique according to claim 1 is characterized in that: replenish when recirculated water makes water inventory reduce by 1/10 needs owing to running off in the described step 2; The fluorinated water total amount of at every turn emitting adopts the mode of distillation to reclaim villiaumite and obtain distilled water at 1.3～1.5 tons.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210057660 CN102585206B (en) | 2012-03-07 | 2012-03-07 | Polyether ketone refining process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210057660 CN102585206B (en) | 2012-03-07 | 2012-03-07 | Polyether ketone refining process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102585206A CN102585206A (en) | 2012-07-18 |
| CN102585206B true CN102585206B (en) | 2013-10-30 |
Family
ID=46474492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210057660 Expired - Fee Related CN102585206B (en) | 2012-03-07 | 2012-03-07 | Polyether ketone refining process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102585206B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382689B (en) * | 2017-08-16 | 2023-06-02 | 宜宾天原集团股份有限公司 | Recovery device and method for acetone and diphenyl sulfone in polyether-ether-ketone production process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0779313A2 (en) * | 1995-12-11 | 1997-06-18 | Basf Aktiengesellschaft | Process for purifying polyarylene ethers with water |
| CN102127218A (en) * | 2010-12-16 | 2011-07-20 | 金发科技股份有限公司 | Device and method for purifying high-temperature-resistant resin |
| CN102127219A (en) * | 2011-01-07 | 2011-07-20 | 金发科技股份有限公司 | Method for purifying polyether ketone/polyether sulfone polymers |
| CN102161739A (en) * | 2011-03-08 | 2011-08-24 | 金发科技股份有限公司 | Method for purifying polymer |
-
2012
- 2012-03-07 CN CN 201210057660 patent/CN102585206B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0779313A2 (en) * | 1995-12-11 | 1997-06-18 | Basf Aktiengesellschaft | Process for purifying polyarylene ethers with water |
| CN102127218A (en) * | 2010-12-16 | 2011-07-20 | 金发科技股份有限公司 | Device and method for purifying high-temperature-resistant resin |
| CN102127219A (en) * | 2011-01-07 | 2011-07-20 | 金发科技股份有限公司 | Method for purifying polyether ketone/polyether sulfone polymers |
| CN102161739A (en) * | 2011-03-08 | 2011-08-24 | 金发科技股份有限公司 | Method for purifying polymer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102585206A (en) | 2012-07-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104973638B (en) | Processing technology of high-salt high-concentration organic waste liquid | |
| CN107117755A (en) | A kind of high ammonia-nitrogen wastewater processing and ammonia recovery system and its method | |
| CN103768923B (en) | Multi-stage gradient absorption device and device for low- and medium-concentration dimethylamine waste gas | |
| CN103936220A (en) | Zero discharge treatment process of saline sewage produced by refining | |
| CN107098414B (en) | Low-temperature evaporation device for treating desulfurization wastewater discharge of power plant and discharge process thereof | |
| CN109020031B (en) | Evaporation concentration system based on thermal compression | |
| CN211445385U (en) | Contain organic solvent's salt waste water evaporation equipment | |
| CN104787823A (en) | Yeast wastewater zero discharge treatment method | |
| CN103253819B (en) | Production technology for treating ternary-monomer wastewater and extracting sodium sulfate | |
| CN110054164A (en) | A kind of dilute sulfuric acid system for concentrating and recycling | |
| CN107596706A (en) | A kind of steam condensation evaporation technology and device | |
| CN102443122B (en) | Production method for refining polyetheretherketone | |
| CN102585206B (en) | Polyether ketone refining process | |
| CN113813623A (en) | MVR concentration and rectification system and recovery method of DMAC waste liquid | |
| CN203754551U (en) | Device for recycling and treating waste water produced during preparation of decanedioic acid by utilizing castor oil | |
| CN104098214B (en) | Containing wastewater from catalyst treatment system | |
| CN208500637U (en) | A kind of processing unit of high sodium sulfate salt high-COD waste water | |
| CN205170589U (en) | High corruption contains useless evaporation of water crystallization process system of salt | |
| CN209602432U (en) | The production system of paraformaldehyde | |
| CN208856938U (en) | A kind of desulfurization wastewater concentration structure | |
| CN206887263U (en) | One kind plating Chrome-free roughening chemical solution purification reclaiming system | |
| CN201906471U (en) | Vacuum concentration device for diluted acid | |
| CN208776344U (en) | A kind of dewaterer for wastewater treatment | |
| CN208814820U (en) | A kind of high-concentration waste emulsification liquid processing device | |
| CN208107657U (en) | Low concentration N-Methyl pyrrolidone transport device in a kind of recycling waste water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131030 Termination date: 20140307 |