CN102702478A - Salt extracting method in production process of epoxy resin - Google Patents
Salt extracting method in production process of epoxy resin Download PDFInfo
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- CN102702478A CN102702478A CN2012101463482A CN201210146348A CN102702478A CN 102702478 A CN102702478 A CN 102702478A CN 2012101463482 A CN2012101463482 A CN 2012101463482A CN 201210146348 A CN201210146348 A CN 201210146348A CN 102702478 A CN102702478 A CN 102702478A
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Abstract
The invention discloses a method for directly extracting salt in a production process of epoxy resin, comprising the following operation steps: step 1 of extracting and separating by a condensation kettle; step 2) of re-extracting; step 3) of over-polymerizing and neutralizing; step 4) of washing and recovering; and step 5) of extracting salt. The technical proposal disclosed by the invention overcomes the defects that investment is huge, and operation and maintenance cost is high in process for extracting salt through multiple-effect evaporation, and solvents generated in a refining process of epoxy resin and saturated salt water generated in an extraction process of crystal salt are recycled so as to reduce total discharge capacity of waste liquors; various indexes of crystal salt extracted by the process meet industrial salt standard GB/T5462-2003.
Description
Technical field
The present invention relates to a kind of in production processes such as epoxy resin the fast and convenient method of carrying salt (sodium-chlor).
Background technology
Technical background: also a certain amount of brilliant salt, a small amount of polymers (aged resin) etc. of crossing in the synthetic bullion epoxy resin that obtains of epoxy resin because except primary product epoxy resin; In order to obtain high-quality epoxy resin finished product; Must make with extra care bullion epoxy resin; To remove the impurity such as salt in the bullion epoxy resin; The method of the removal salt that generally adopts at present is with clear water brilliant salt to be dissolved earlier, then with the epoxy resin extracting and separating, again salt solution is carried out preparing Industrial Salt through multi-effect evaporating device after the pre-treatment.But this method exists equipment to have high input, a great problem that energy consumption is high.Add solvent and saturated brine in the also oriented in addition bullion epoxy resin, carry out separated and dissolved, the brilliant salt that obtains and saturated brine are carried out steps such as spinning, oven dry, calcination obtain Industrial Salt; But technology relative complex; Operation is loaded down with trivial details, and what add in the crude salt treating process is fresh solvent, and the solvent makeup amount is big; Directly influence solvent recycling in the epoxy resin treating process, be unfavorable for energy-saving and emission-reduction; Its three this method is taken out most of salt of epoxy resin production process, does not remove but still there is to make with extra care the salt solution of adding the alkali generation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of and utilizes to carry a salt oven; Saved the vaporizer of multiple-effect evaporation, the infusion of financial resources of minimizing equipment, extraction process is simple and convenient; Do not influence the production capacity of whole device again, and put forward the salt method in the relatively low epoxy resin production process of processing cost.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is: put forward the salt method in a kind of epoxy resin production process, its operation steps is:
1) condensation still extracting and separating: after the condensation of bullion epoxy resin finishes, in the condensation still, add extracting mother liquid and bullion salt solution, temperature is controlled at 80 ± 5 ℃; Stir 15～30min, stop to stir, leave standstill 20～30min layering; The superiors are the bullion epoxy resin solution; The second layer was polymers (a veteran resin), and the 3rd layer is saturated brine, and orlop is brilliant salt; Undermost brilliant salt and trilaminar saturated brine be transferred to carry salt oven pending; In the condensation still, add bullion salt solution again; Under 80 ± 5 ℃ of conditions, stir 5～15min; Stop to stir, leave standstill 30～40min, undermost brilliant salt and trilaminar saturated brine are transferred to once more carry in the salt oven; After the crossing polymers (veteran resin) and leave standstill 5～10min again of the bullion epoxy resin solution of the first layer and the second layer, will cross polymers (veteran resin) and bullion epoxy resin solution and be transferred to refining kettle and make with extra care;
Said extracting mother liquid is a step 2) and step 3) be separated in the extracting mother liquid groove extraction solvent with had the salt solution of polymers (veteran resin), the adding quality of extracting mother liquid and the ratio of epoxy resin Theoretical Mass are 0.3～0.5:1; The each bullion brine quality that adds and the ratio of epoxy resin Theoretical Mass are 0.2～0.3:1;
2) reextraction: add recovered solvent in the epoxy resin production treating process in carrying salt oven; 10～30min is stirred in 80 ± 5 ℃ of temperature controls, stops to stir; Leave standstill 30～40min; Be transferred to the extracting mother liquid groove after the upper strata extraction solvent is cooled to 60 ± 30 ℃, be transferred to the bullion saline after will having brine refrigeration to 65 ± 40 ℃ of polymers (veteran resin) again, carry residue saturated brine and brilliant salt in the salt oven;
In the whole reextraction process, condensing and recycling is evaporated the liquid that, and the solvent in the recovering liq is gone to the extracting mother liquid groove, and waste water is discharged;
Said extraction solvent is that solubility parameters is at 20～18 (J/cm
2)
1/2Between solvent, the ratio of extraction solvent quality and epoxy resin Theoretical Mass is 0.2～0.5:1;
3) gather neutralization excessively: in carrying salt oven, add extraction solvent and saturated brine; Temperature is controlled at 80 ± 5 ℃; Adding quality percentage composition is 32 ~ 48% aqueous sodium hydroxide solution (liquid caustic soda), stirs 30～40min, feeds saturation steam; Steam flow is controlled at 20～150Kg/h, keeps 15～20min; Adding quality percentage composition is 20%～30% hydrochloric acid, and tracking sampling detects the pH value of putting forward in the salt oven, regulates pH=7; Stop that saturation steam feeds and stir, leave standstill 10～20min, be transferred to extracting mother liquid groove and bullion saline respectively behind upper strata solvent and brine refrigeration to 30 ~ 60 that had polymers (veteran resin) ℃;
The ratio of said extraction solvent quality and epoxy resin Theoretical Mass is 0.2～0.5:1; The ratio of said saturated brine quality and epoxy resin Theoretical Mass is 0.1～0.2:1; Said quality percentage composition is that 32% the aqueous sodium hydroxide solution quality and the ratio of epoxy resin Theoretical Mass are 0.01～0.05:1;
4) washing and recycling: in carrying salt oven, add saturated brine, stir, pressure-controlling is at-98 ± 2KPa; Feed saturation steam, the liquid level of control steam flow 10～50Kg/h, 105 ± 5 ℃ of temperature, surge tank is no more than 70%, and the time is kept 30～60min; Remove vacuum then, stop to feed saturation steam, be cooled to 45 ± 5 ℃; Stop to stir, leave standstill 30～60min, the upper strata saturated brine is transferred to the bullion saline after being cooled to 45 ± 5 ℃;
The saturated brine washing process: under the normal pressure, in carrying salt oven, add saturated brine again, stir, feed saturation steam, steam flow is controlled at 10～50Kg/h; Temperature is controlled at 45 ± 5 ℃, and the time is kept 5～10min, stops to feed saturation steam, leaves standstill 30～60min, is transferred to the crude salt tank after the upper strata saturated brine is cooled to 45 ± 5 ℃; Repeat water-insoluble quality percentage composition≤0.2% of saturated brine washing process in the isolated saturated brine of washing;
Said saturated brine quality and epoxy resin Theoretical Mass ratio are 0.1～0.3:1;
5) carry salt: residue saturated brine and brilliant salt after step 4) washing is accomplished, leave standstill and be transferred to the tripping device dehydration after being cooled to 45 ± 5 ℃, dry then Industrial Salt; Separate the saturated brine that obtains and be transferred to the saturated salt tank.
In the said step 1), the extracting mother liquid that adds first is the extraction solvent that reclaims in the epoxy resin treating process; The bullion salt solution that adds first is to add the saturated brine that produces behind the alkali in the epoxy resin treating process.
Said step 2) waste water of phase splitter discharge is delivered to three wastes biochemical treatment.
In the said extraction solvent, solubility parameters is at 20～18 (J/cm
2)
1/2Between solvent, be preferably toluene or MIBK.
In the said step 4), surge tank is reclaimed the liquid obtain through the phase splitter phase-splitting, upper strata high boiling material collection and treatment, lower floor's waste water are delivered to the three wastes and are handled.
This method compared with prior art, beneficial effect of the present invention is: technical scheme disclosed by the invention overcome adopt that multiple-effect evaporation carries that the salt infusion of financial resources is big, operation and the high shortcoming of maintenance cost, also avoided limiting simultaneously the production capacity of whole epoxy resin device because of extracting and separating; And the solvent that produces in the abundant recycle epoxy resin treating process; Reduced the magnitude of recruitment of fresh solvent, met the energy-saving and emission-reduction requirement, and overcome in the epoxy resin treating process because of lacking the emulsion that the fresh solvent magnitude of recruitment brings; Minimizing is because of handling the financial loss that emulsifying resins brings; This method is also with the salt water circulation use in the treating process, reduces the brinish total release, and gathers the micro-resin that method will be included in saturated brine and gathered through crossing; Reduced because of the molten influence of a small amount of epoxy resin brilliant salt quality; Control the pH value of brilliant salt through neutralizing treatment, separate with the organism that boils attached to the water-soluble solvent on brilliant salt surface and height being dissolved in saturated brine, reduced because of the influence of organism of boiling of water-soluble solvent and height to the salt quality through bubbling and negative pressure; Through the repeated washing of saturated brine, washing effect is good again.
Description of drawings
Fig. 1 is the process flow sheet of embodiment.
Embodiment
Below in conjunction with embodiment the present invention is described further, but can not be as limitation of the present invention.
Embodiment 1
Theoretical amount of resin: 12000Kg
1) after end is reclaimed in the condensation of condensation still, add extracting mother liquid (the refining toluene 5000Kg+ saturated brine 2500Kg that reclaims of epoxy resin) at bullion epoxy resin, temperature is controlled at 82 ℃～83 ℃; Stir 15min, stop to stir, leave standstill 30min; Brilliant salt of orlop and saturated brine be transferred to carry salt oven pending, remaining bullion epoxy resin solution with cross polymers (veteran resin) adding 2500Kg saturated brine, temperature is controlled at 80 ℃～83 ℃; Stir 5min, stop to stir, leave standstill 30min; To descend layer crystal salt and saturated brine to be transferred to once more and carry salt oven; The bullion epoxy resin solution with cross polymers (veteran resin), leave standstill 10min, earlier crossing polymers (aged resin) incision refining kettle; Switch to the later process extraction through refining kettle crossing polymers (aged resin), it is refining that remaining bullion epoxy resin solution all moves to refining kettle;
2) open the condenser cooling water of carrying salt oven, surge tank terminal valve, the valve between phase splitter to the extracting mother liquid groove automatically; Cut off the valve between phase splitter and the high boiling material, the middle 3000Kg of adding toluene in carrying salt oven (the refining toluene that reclaims of crude resin), 80 ℃～83 ℃ of temperature controls; Stir 30min; Stop to stir, leave standstill 30min, open the refrigerating unit water coolant; Upper toluene resin, mistake polymers (aged resin) are delivered in the extracting mother liquid groove through the apparatus for supercooling transfer, and the salt solution that the middle layer had polymers is transferred to the bullion saline through refrigerating unit.
3) add 5100Kg toluene and saturated 2000Kg saturated brine, temperature is controlled at 80 ℃～83 ℃, adds 32Wt.% aqueous sodium hydroxide solution 250Kg and (adds alkali speed: 30Kg/min); Stir 30min; Feed saturation steam, steam flow is controlled at 10Kg/h, keeps 30min.Stop to feed saturation steam, (add sour speed: 20Kg/min), whenever a pH value is surveyed in sampling after one minute, stops to add acid during to pH=7 slowly to add 30Wt.% hydrochloric acid.Stop to stir, leave standstill 10min, upper toluene is transferred to the extracting mother liquid groove through refrigerating unit, the salt solution of crossing polymers (aged resin) is transferred to the bullion saline through refrigerating unit;
The actual add-on 356Kg of described 30Wt.% hydrochloric acid.
4) add saturated brine 1200Kg, open and stir, cut off the valve between surge tank and the phase splitter, open vacuum valve, pressure-controlling-96～-98KPa, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 102～105 ℃, observes surge tank, behind the 40min, removes vacuum, is cooled to 45 ℃, stops to stir, and leaves standstill 60min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.Open the valve between phase splitter to the high boiling material, slowly open the valve between surge tank to the phase splitter, reclaim upper strata high boiling material, lower floor's waste water.
Add saturated brine 1200Kg, open and stir, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.
Secondary adds saturated brine 1200Kg, opens and stirs, and feeds saturation steam, and steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit, detects the saturated brine water-insoluble 0.2% after washing.
5) will remain saturated brine and brilliant salt is transferred to automatic high speed centrifuge dewatering, drying, saturated brine desaturation saline is subsequent use, separate brilliant salt 3500Kg.
To above-mentioned brilliant salt analysis, the result is (said numerical value is the quality percentage composition) as follows:
Embodiment 2
Theoretical amount of resin: 6700Kg
1) after end is reclaimed in the condensation of condensation still, add extracting mother liquid (the refining toluene 3000Kg+ saturated brine 1500Kg that reclaims of epoxy resin) at bullion epoxy resin, temperature is controlled at 82 ℃～83 ℃; Stir 15min, stop to stir, leave standstill 30min; Brilliant salt of orlop and saturated brine be transferred to carry salt oven pending, remaining bullion epoxy resin solution with cross polymers (veteran resin) adding 1500Kg saturated brine, temperature is controlled at 80 ℃～83 ℃; Stir 5min, stop to stir, leave standstill 30min; To descend layer crystal salt and saturated brine to be transferred to once more and carry salt oven; The bullion epoxy resin solution with cross polymers (veteran resin), leave standstill 10min, earlier crossing polymers (aged resin) incision refining kettle; Switch to the later process extraction through refining kettle crossing polymers (aged resin), it is refining that remaining bullion epoxy resin solution all moves to refining kettle;
2) open the condenser cooling water of carrying salt oven, surge tank terminal valve, the valve between the extracting mother liquid groove of phase splitter automatically; Cut off the valve between phase splitter and the high boiling material, the middle 2500Kg of adding toluene in carrying salt oven (the refining toluene that reclaims of crude resin), 80 ℃～83 ℃ of temperature controls; Stir 30min; Stop to stir, leave standstill 30min, open the refrigerating unit water coolant; Upper toluene resin, mistake polymers (aged resin) apparatus for supercooling are shifted and deliver to the extracting mother liquid groove, and the salt solution that the middle layer had polymers is transferred to the bullion saline through refrigerating unit.
3) add 1500Kg toluene and saturated 1200Kg saturated brine, temperature is controlled at 80 ℃～83 ℃, adds 32Wt.% aqueous sodium hydroxide solution 85Kg and (adds alkali speed: 30Kg/min); Stir 30min; Feed saturation steam, steam flow is controlled at 10Kg/h, keeps 30min.Stop to feed saturation steam, (add sour speed: 20Kg/min), whenever a pH value is surveyed in sampling after one minute, stops to add acid during to pH=7 slowly to add 30Wt.% hydrochloric acid.Stop to stir, leave standstill 10min, upper toluene is transferred to the extracting mother liquid groove through refrigerating unit, the salt solution of crossing polymers (aged resin) is transferred to the bullion saline through refrigerating unit;
The actual add-on 125Kg of described 30Wt.% hydrochloric acid.
4) add saturated brine 1000Kg, open and stir, cut off the valve between surge tank and the phase splitter, open vacuum valve, pressure-controlling-96～-98KPa, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 102～105 ℃, observes surge tank, behind the 40min, removes vacuum, is cooled to 45 ℃, stops to stir, and leaves standstill 60min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.Open the valve between phase splitter and the high boiling material, slowly open the valve between surge tank and the phase splitter, reclaim upper strata high boiling material, lower floor's waste water.
Add saturated brine 1000Kg, open and stir, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.
Secondary adds saturated brine 1000Kg, opens and stirs, and feeds saturation steam, and steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit, detects the saturated brine water-insoluble quality percentage composition 0.2% after washing.
5) will remain saturated brine and brilliant salt is transferred to automatic high speed centrifuge dewatering, drying, saturated brine desaturation saline is subsequent use, separate brilliant salt 2200Kg.
To above-mentioned brilliant salt analysis, the result is (said numerical value is the quality percentage composition) as follows:
Embodiment 3
Theoretical amount of resin: 9400Kg
1) after end is reclaimed in the condensation of condensation still, add extracting mother liquid (the refining MIBK 4700Kg+ saturated brine 1620Kg that reclaims of epoxy resin) at bullion epoxy resin, temperature is controlled at 82 ℃～83 ℃; Stir 15min, stop to stir, leave standstill 30min; Brilliant salt of orlop and saturated brine be transferred to carry salt oven pending, remaining bullion epoxy resin solution with cross polymers (veteran resin) adding 1620Kg saturated brine, temperature is controlled at 80 ℃～83 ℃; Stir 5min, stop to stir, leave standstill 30min; To descend layer crystal salt and saturated brine to be transferred to once more and carry salt oven; The bullion epoxy resin solution with cross polymers (veteran resin), leave standstill 10min, earlier crossing polymers (aged resin) incision refining kettle; Switch to the later process extraction through refining kettle crossing polymers (aged resin), it is refining that remaining bullion epoxy resin solution all moves to refining kettle;
2) open the condenser cooling water of carrying salt oven, surge tank terminal valve, the valve between phase splitter to the extracting mother liquid groove automatically; Cut off the valve between phase splitter and the high boiling material, the middle 2700Kg of adding MIBK in carrying salt oven (the refining MIBK that reclaims of crude resin), 80 ℃～83 ℃ of temperature controls; Stir 30min; Stop to stir, leave standstill 30min, open the refrigerating unit water coolant; With upper strata MIBK and resin, cross polymers (aged resin) and shift through apparatus for supercooling and deliver in the extracting mother liquid groove, the salt solution that had polymers is transferred to the bullion saline through refrigerating unit.
3) add 2700Kg MIBK and saturated 1080Kg saturated brine, temperature is controlled at 80 ℃～83 ℃, adds 32Wt.% aqueous sodium hydroxide solution 270Kg and (adds alkali speed: 30Kg/min); Stir 30min; Feed saturation steam, steam flow is controlled at 10Kg/h, keeps 30min.Stop to feed saturation steam, (add sour speed: 20Kg/min), whenever a pH value is surveyed in sampling after one minute, stops to add acid during to pH=7 slowly to add 30Wt.% hydrochloric acid.Stop to stir, leave standstill 10min, the upper strata MIBK is transferred to the extracting mother liquid groove through refrigerating unit, the salt solution of crossing polymers (aged resin) is transferred to the bullion saline through refrigerating unit;
The actual add-on 136Kg of described 30Wt.% hydrochloric acid.
4) add saturated brine 1620Kg, open and stir, cut off the valve between surge tank and the phase splitter, open vacuum valve, pressure-controlling-96～-98KPa, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 102～105 ℃, observes surge tank, behind the 40min, removes vacuum, is cooled to 45 ℃, stops to stir, and leaves standstill 60min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.Open the valve between phase splitter to the high boiling material, slowly open the valve between surge tank to the phase splitter, reclaim upper strata high boiling material, lower floor's waste water.
Add saturated brine 1620Kg, open and stir, feed saturation steam, steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit.
Secondary adds saturated brine 1620Kg, opens and stirs, and feeds saturation steam, and steam flow is controlled at 10Kg/h; Temperature is controlled at 50 ℃, and time dimension is held in 5min, stops to feed saturation steam, leaves standstill 30min, and the upper strata saturated brine is transferred to the crude salt tank through refrigerating unit, detects the saturated brine water-insoluble 0.2% after washing.
5) will remain saturated brine and brilliant salt is transferred to automatic high speed centrifuge dewatering, drying, saturated brine desaturation saline is subsequent use, separate brilliant salt 1500Kg.
To above-mentioned brilliant salt analysis, the result is (said numerical value is the quality percentage composition) as follows:
Claims (5)
1. directly extract the method for salt in the epoxy resin production process, its operation steps is:
1) condensation still extracting and separating: after the condensation of bullion epoxy resin finishes, in the condensation still, add extracting mother liquid and bullion salt solution, temperature is controlled at 80 ± 5 ℃; Stir 15～30min, stop to stir, leave standstill 20～30min layering; The superiors are the bullion epoxy resin solution; The second layer was a polymers, and the 3rd layer is saturated brine, and orlop is brilliant salt; Undermost brilliant salt and trilaminar saturated brine be transferred to carry salt oven pending; In the condensation still, add bullion salt solution again; Under 80 ± 5 ℃ of conditions, stir 5～15min; Stop to stir, leave standstill 30～40min, undermost brilliant salt and trilaminar saturated brine are transferred to once more carry in the salt oven; After the crossing polymers and leave standstill 5～10min again of the bullion epoxy resin solution of the first layer and the second layer, will cross polymers and bullion epoxy resin solution and be transferred to refining kettle and make with extra care;
Said extracting mother liquid is a step 2) and step 3) be separated in the extracting mother liquid groove extraction solvent with had the salt solution of polymers, the adding quality of extracting mother liquid and the ratio of epoxy resin Theoretical Mass are 0.3～0.5:1; The each bullion brine quality that adds and the ratio of epoxy resin Theoretical Mass are 0.2～0.3:1;
2) reextraction: add recovered solvent in the epoxy resin production treating process in carrying salt oven; 10～30min is stirred in 80 ± 5 ℃ of temperature controls, stops to stir; Leave standstill 30～40min; Be transferred to the extracting mother liquid groove after the upper strata extraction solvent is cooled to 60 ± 30 ℃, be transferred to the bullion saline after will having brine refrigeration to 65 ± 40 ℃ of polymers again, carry residue saturated brine and brilliant salt in the salt oven;
In the above-mentioned reextraction process, condensing and recycling is evaporated the liquid that, and the solvent in the recovering liq is gone to the extracting mother liquid groove, and waste water is discharged;
Said extraction solvent is that solubility parameters is at 20～18 (J/cm
2)
1/2Between solvent, the ratio of extraction solvent quality and epoxy resin Theoretical Mass is 0.2～0.5:1;
3) gather neutralization excessively: in carrying salt oven, add extraction solvent and saturated brine, temperature is controlled at 80 ± 5 ℃, and adding quality percentage composition is 32 ~ 48% aqueous sodium hydroxide solution; Stir 30～40min; Feed saturation steam, steam flow is controlled at 20～150Kg/h, keeps 15～20min; Adding quality percentage composition is 20%～30% hydrochloric acid, and the pH value in the salt oven is put forward in tracking sampling, detection, regulates pH=7; Stop that saturation steam feeds and stir, leave standstill 10～20min, be transferred to extracting mother liquid groove and bullion saline respectively behind upper strata solvent and brine refrigeration to 30 ~ 60 that had polymers ℃;
The ratio of said extraction solvent quality and epoxy resin Theoretical Mass is 0.2～0.5:1; The ratio of said saturated brine quality and epoxy resin Theoretical Mass is 0.1～0.2:1; Said quality percentage composition is that 32% the aqueous sodium hydroxide solution quality and the ratio of epoxy resin Theoretical Mass are 0.01～0.05:1;
4) washing and recycling: in carrying salt oven, add saturated brine, stir, pressure-controlling is at-98 ± 2KPa; Feed saturation steam, the liquid level of control steam flow 10～50Kg/h, 105 ± 5 ℃ of temperature, surge tank is no more than 70%, and the time is kept 30～60min; Remove vacuum then, stop to feed saturation steam, be cooled to 45 ± 5 ℃; Stop to stir, leave standstill 30～60min, the upper strata saturated brine is transferred to the bullion saline after being cooled to 45 ± 5 ℃;
The saturated brine washing process: under the normal pressure, in carrying salt oven, add saturated brine again, stir, feed saturation steam, steam flow is controlled at 10～50Kg/h; Temperature is controlled at 45 ± 5 ℃, and the time is kept 5～10min, stops to feed saturation steam, leaves standstill 30～60min, is transferred to the crude salt tank after the upper strata saturated brine is cooled to 45 ± 5 ℃; Repeat water-insoluble quality percentage composition≤0.2% of saturated brine washing process in the isolated saturated brine of washing;
Said saturated brine quality and epoxy resin Theoretical Mass ratio are 0.1～0.3:1;
5) carry salt: residue saturated brine and brilliant salt after step 4) washing is accomplished, leave standstill and be transferred to the tripping device dehydration after being cooled to 45 ± 5 ℃, dry then Industrial Salt; Separate the saturated brine that obtains and be transferred to the saturated salt tank.
2. according to the method for directly extracting salt in the said a kind of epoxy resin production process of claim 1, it is characterized in that: in the said step 1), the extracting mother liquid that adds first is the extraction solvent that reclaims in the epoxy resin treating process; The bullion salt solution that adds first is to add the saturated brine that produces behind the alkali in the epoxy resin treating process.
3. according to the method for directly extracting salt in the said a kind of epoxy resin production process of claim 1, it is characterized in that: said step 2) waste water of phase splitter discharge is delivered to three wastes biochemical treatment.
4. according to the method for directly extracting salt in the said a kind of epoxy resin production process of claim 1, it is characterized in that: in the said extraction solvent, solubility parameters is at 20～18 (J/cm
2)
1/2Between solvent, be preferably toluene or MIBK.
5. according to the method for directly extracting salt in the said a kind of epoxy resin production process of claim 1; It is characterized in that: in the said step 4); Surge tank is reclaimed the liquid obtain through the phase splitter phase-splitting, and upper strata high boiling material collection and treatment, lower floor's waste water are delivered to the three wastes and are handled.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105754071A (en) * | 2016-02-29 | 2016-07-13 | 宏昌电子材料股份有限公司 | Preparation technology of bisphenol fluorene epoxy resin |
| CN111547925A (en) * | 2020-06-16 | 2020-08-18 | 无锡厚德石化工程设计有限公司 | Pretreatment process of high-salinity wastewater in epoxy resin production |
| CN118085229A (en) * | 2024-04-19 | 2024-05-28 | 东方飞源(山东)电子材料有限公司 | Epoxy resin refining process for reducing toluene wastewater and byproduct industrial salt |
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| CN101117258A (en) * | 2007-07-24 | 2008-02-06 | 浙江大学 | Method for treating epoxy resin waste-water with high alkalinity, high salt and high content of organics |
| US20100193443A1 (en) * | 2007-08-23 | 2010-08-05 | Chaudhary Sunil K | Total organic carbon (toc) reduction in brine via chlorinolysis |
| CN101481190A (en) * | 2009-02-10 | 2009-07-15 | 杭州水处理技术研究开发中心有限公司 | Process for treating saponification wastewater by chlorohydrination |
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| CN105754071A (en) * | 2016-02-29 | 2016-07-13 | 宏昌电子材料股份有限公司 | Preparation technology of bisphenol fluorene epoxy resin |
| CN111547925A (en) * | 2020-06-16 | 2020-08-18 | 无锡厚德石化工程设计有限公司 | Pretreatment process of high-salinity wastewater in epoxy resin production |
| CN118085229A (en) * | 2024-04-19 | 2024-05-28 | 东方飞源(山东)电子材料有限公司 | Epoxy resin refining process for reducing toluene wastewater and byproduct industrial salt |
| CN118085229B (en) * | 2024-04-19 | 2024-06-21 | 东方飞源(山东)电子材料有限公司 | Epoxy resin refining process for reducing toluene wastewater and byproduct industrial salt |
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