CN103396327B - Preparation technology of 2, 4-diamino-phenoxyethanol hydrochloride - Google Patents
Preparation technology of 2, 4-diamino-phenoxyethanol hydrochloride Download PDFInfo
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- CN103396327B CN103396327B CN201310348541.9A CN201310348541A CN103396327B CN 103396327 B CN103396327 B CN 103396327B CN 201310348541 A CN201310348541 A CN 201310348541A CN 103396327 B CN103396327 B CN 103396327B
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Abstract
The invention discloses a preparation technology of 2, 4-diamino-phenoxyethanol hydrochloride. The preparation technology is characterized in that 2, 4-dinitrochlorobenzene serving as a main raw material is subjected to condensation with glycol under an alkaline condition, then is hydrogenated and finally is salified with hydrochloric acid to obtain the 2, 4-diamino-phenoxyethanol hydrochloride. The preparation technology comprises a condensation working section, a hydrogenation reduction working section and a salt formation and precipitation working section. The preparation technology disclosed by the invention has the advantages that part of materials are recycled and reused, the amount of generated waste materials is reduced, the clean production is realized, the cost is saved, and the yield is high and stable.
Description
Technical field
The present invention relates to a kind of manufacturing process of hydrochloride, particularly a kind of manufacturing process of 2,4-diaminophenoxy ethanol hydrochloride.
Background technology
2,4-diaminophenoxy ethanol hydrochloride is mainly used as hair dye or medicine intermediate, is widely used in actual life.
But the manufacturing process system of existing 2,4-diaminophenoxy ethanol hydrochlorides not exclusively, and materials are disposable, can not realize recycling, create very large waste, and due to the chemical property of filtrate, causing can to environment.
Summary of the invention
Goal of the invention: the object of the invention is to solve the manufacturing process that prior art does not have 2,4-concrete diaminophenoxy ethanol hydrochlorides, and the problem of existing manufacturing process filtrate waste.
Technical scheme: the invention provides following technical scheme: a kind of manufacturing process of 2,4-diaminophenoxy ethanol hydrochloride, comprises the following steps:
1) condensation workshop section
Open vacuum system, ethylene glycol is sucked in pot, then open stirring, after sucking the DNFB dissolved in advance, again suck ethylene glycol, keep temperature 60 ~ 80 DEG C; Open manhole, dropped into by sodium carbonate in still, build manhole, open emptying valve, open water rushes pump and vacuumizes in still; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, after water of condensation all drains, then switch to trap; Keep temperature 100 ~ 140 DEG C, pH value 7.5 ~ 8, closes water after draining carbonic acid gas and rushes pump, stirs 4 ~ 6 hours; Insulation reaction terminates, sampling be TLC analyze qualified after, add 1000kg water, be warming up to 90 ~ 95 DEG C, stir 1 hour; Leave standstill 30 minutes, then supernatant liquid is sucked continuation cooling in cooling reactor, when temperature in the kettle is down to 30 ~ 40 DEG C, switch chilled brine, continue to be cooled to 10 ~ 20 DEG C, blowing suction filtration, obtain condensation material; Suction filtration terminates, and filter cake is with ionized water rinsing to neutral, and point secondary centrifuging, centrifugal 1 ~ 2 hour at every turn, filtrate suction was reclaimed in pot, and centrifugal end is weighed.
2) hydrogenating reduction workshop section
Condensation material is added DMF and palladium charcoal, mixing and stirring; Hydrogenation still vacuumizes, and the material mixed is sucked hydrogenation still; Hydrogenation still is replaced, is replaced rear increase still internal pressure to 12kg/cm
2, start magnetic stirring vessel and stir; Keep temperature 40 ~ 60 DEG C, stir 1 ~ 2 hour; Releasing hydrogen gas, replaces into nitrogen 10kg, opens and stirs cooling pan filtration; Hydrogenation still is replaced, makes binder and prepare; Feed liquid nitrogen pressure in hydrogenation still is slowly depressed in suction filtration bucket and carries out suction filtration; Filtrate sucks still kettle, and palladium charcoal is cleaned with DMF and reclaimed.
3) salify analysis of material workshop section
Add feed liquid suction still kettle, after exhausting, heat temperature raising carries out underpressure distillation, distills and terminate when temperature in the kettle adds to 120 DEG C; Open cooling water valve, temperature in the kettle is cooled to 40 ~ 50 DEG C; Open water rushes pump and vacuumizes still kettle, water and hydrochloric acid is sucked still kettle, stirs 30 minutes; Close water and rush pump, add gac; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, keep temperature 88 ~ 90 DEG C, stir decolouring 1 hour; Decolouring terminates, and filter immediately, filtrate enters finished product still kettle, and gac turns over and washes once simultaneously, then uses 60 ~ 80 DEG C of water rinses to pH value 3 ~ 4, and washing water water rushes pump and sucks still kettle; When still kettle stirring rake encounters filtrate, open underpressure distillation, rotating speed keeps 1450 rpms; When there being material to separate out in still, speed governing 1050 rpms, continues distillation 1 hour, then closes distillation, speed governing 600 rpms, and chuck enters tap water cooling, rotating speed 530 turns during cooling; Temperature in the kettle is cooled to less than 30 ~ 40 DEG C, and chuck uses chilled brine instead, treats that temperature in the kettle is cooled to 0 DEG C, continues stirring 1 hour; Stir and terminate blowing suction filtration, after draining points three times centrifugal, centrifugal 1 ~ 2 hour at every turn; Suction filtration filtrate recovery, mark is carried out in centrifugal end, proceeds to drying section and finally obtains 2,4-diaminophenoxy ethanol hydrochloride.
As optimization, the lower floor's by product obtained after described condensation workshop section leaves standstill 30 minutes, after supernatant liquid sucks, adds mother liquor and is warming up to 90 DEG C, stir 15 minutes, blowing suction filtration, filtrate sucks cooling reactor and is cooled to 15 DEG C, filter residue rinsed clean, barrelling after centrifuge dripping, and carry out mark.
As optimization, in described hydrogenating reduction workshop section hydrogenation process, regulate hydrogen valve, keep still internal pressure 12kg/cm
2.
As optimization, the underpressure distillation of described salify analysis of material workshop section keeps vacuum tightness 0.085MPa, automatic steam control 0.1MPa.
As optimization, during described salify analysis of material workshop section cooling, cooling pan not emptying, keeps vacuum tightness.
As optimization, described salify analysis of material workshop section whizzer need first with the hydrochloric acid water rinsing that the PH of 5kg is 1.
As optimization, described condensation workshop section filter residue rinsing pH value keeps 7 ~ 7.5.
Beneficial effect: the present invention compared with prior art: the invention provides concrete 2; the manufacturing process of 4-diaminophenoxy ethanol hydrochloride; for existing 2; the production supplying method of 4-diaminophenoxy ethanol hydrochloride; and manufacturing process provided by the invention does not have the character affecting filtrate due to production process; so finally can the carrying out blowing suction filtration and centrifugally to recycle filtrate of each workshop section; this can save very large cost in large-scale industrial production; and decrease the waste material of generation; achieve cleaner production, protect environment.
Embodiment
Embodiment 1
Carry out production 2,4-diaminophenoxy ethanol hydrochloride
1) condensation workshop section
Open vacuum system, 400kg ethylene glycol is sucked in pot, then opens stirring, suck the 160kg2 dissolved in advance, after 4-dinitrochlorobenzene, again suck 200kg ethylene glycol, keep temperature 60 C; Open manhole, dropped in still by 45kg sodium carbonate, build manhole, open emptying valve, open water rushes pump and vacuumizes in still; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, after water of condensation all drains, then switch to trap; Keep temperature 100 DEG C, pH value 7.5, closes water after draining carbonic acid gas and rushes pump, stirs 4 hours; Insulation reaction terminates, sampling be TLC analyze qualified after, add 1000kg water, be warming up to 90 DEG C, stir 1 hour; Leave standstill 30 minutes, then supernatant liquid is sucked continuation cooling in cooling reactor, when temperature in the kettle is down to 30 DEG C, switch chilled brine, continue to be cooled to 10 DEG C, blowing suction filtration, obtain condensation material 165kg; Suction filtration terminates, and filter cake to neutral, divides secondary centrifuging with ionized water rinsing, centrifugal 1 hour at every turn, filtrate suction was reclaimed in pot, and centrifugal end is weighed, the standing lower floor's by product obtained for 30 minutes, after supernatant liquid sucks, adds mother liquor and is warming up to 90 DEG C, stir 15 minutes, blowing suction filtration, filtrate sucks cooling reactor and is cooled to 15 DEG C, filter residue rinsed clean, and filter residue rinsing pH value keeps 7, barrelling after centrifuge dripping, and carry out mark.
2) hydrogenating reduction workshop section
165kg condensation material is added 560kgDMF and 2.7kg palladium charcoal, mixing and stirring; Hydrogenation still vacuumizes, and the material mixed is sucked hydrogenation still; Hydrogenation still is replaced, is replaced rear increase still internal pressure to 12kg/cm
2, start magnetic stirring vessel and stir, in hydrogenation process, regulate hydrogen valve, keep still internal pressure 12kg/cm
2; Keep temperature 40 DEG C, stir 1 hour; Releasing hydrogen gas, replaces into nitrogen 10kg, opens and stirs cooling pan filtration; Hydrogenation still is replaced, makes binder and prepare; Feed liquid nitrogen pressure in hydrogenation still is slowly depressed in suction filtration bucket and carries out suction filtration; Filtrate sucks still kettle, and palladium charcoal is cleaned with DMF and reclaimed.
3) salify analysis of material workshop section
Add feed liquid suction still kettle, after exhausting, heat temperature raising carries out underpressure distillation, and distill when temperature in the kettle adds to 120 DEG C and terminate, underpressure distillation keeps vacuum tightness 0.085MPa, automatic steam control 0.1MPa; Open cooling water valve, temperature in the kettle is cooled to 40 DEG C; Open water rushes pump and vacuumizes still kettle, 1000kg water and 186kg hydrochloric acid is sucked still kettle, stirs 30 minutes; Close water and rush pump, add 60kg gac; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, keep temperature 88 DEG C, stir decolouring 1 hour; Decolouring terminates, and filter immediately, filtrate enters finished product still kettle, and gac turns over and washes once simultaneously, then is 3 with 60 DEG C of water rinses to pH value, and washing water water rushes pump and sucks still kettle; When still kettle stirring rake encounters filtrate, open underpressure distillation, rotating speed keeps 1450 rpms; When there being material to separate out in still, speed governing 1050 rpms, continues distillation 1 hour, then closes distillation, speed governing 600 rpms, and chuck enters tap water cooling, rotating speed 530 turns during cooling, and cooling pan not emptying during cooling keeps vacuum tightness; Temperature in the kettle is cooled to less than 30 DEG C, and chuck uses chilled brine instead, treats that temperature in the kettle is cooled to 0 DEG C, continues stirring 1 hour; Stir terminate whizzer need first with the hydrochloric acid water rinsing that the PH of 5kg is 1, blowing suction filtration, drain after divide three times centrifugal, centrifugal 1 hour at every turn; Suction filtration filtrate recovery, mark is carried out in centrifugal end, proceeds to drying section and finally obtains 2,4-diaminophenoxy ethanol hydrochloride, 2,4-diaminophenoxy ethanol hydrochloric acid salts contg≤99.07, yield 91%, the filtrate rate of recovery 90%.
Embodiment 2
Carry out production 2,4-diaminophenoxy ethanol hydrochloride
1) condensation workshop section
Open vacuum system, 400kg ethylene glycol is sucked in pot, then opens stirring, suck the 160kg2 dissolved in advance, after 4-dinitrochlorobenzene, again suck 200kg ethylene glycol, keep temperature 70 C; Open manhole, dropped in still by 45kg sodium carbonate, build manhole, open emptying valve, open water rushes pump and vacuumizes in still; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, after water of condensation all drains, then switch to trap; Keep temperature 120 DEG C, pH value 7.5, closes water after draining carbonic acid gas and rushes pump, stirs 5 hours; Insulation reaction terminates, sampling be TLC analyze qualified after, add 1000kg water, be warming up to 92 DEG C, stir 1 hour; Leave standstill 30 minutes, then supernatant liquid is sucked continuation cooling in cooling reactor, when temperature in the kettle is down to 35 DEG C, switch chilled brine, continue to be cooled to 15 DEG C, blowing suction filtration, obtain condensation material 165kg; Suction filtration terminates, and filter cake to neutral, divides secondary centrifuging with ionized water rinsing, centrifugal 1 hour at every turn, filtrate suction was reclaimed in pot, and centrifugal end is weighed, the standing lower floor's by product obtained for 30 minutes, after supernatant liquid sucks, adds mother liquor and is warming up to 90 DEG C, stir 15 minutes, blowing suction filtration, filtrate sucks cooling reactor and is cooled to 15 DEG C, filter residue rinsed clean, and filter residue rinsing pH value keeps 7, barrelling after centrifuge dripping, and carry out mark.
2) hydrogenating reduction workshop section
165kg condensation material is added 560kgDMF and 2.7kg palladium charcoal, mixing and stirring; Hydrogenation still vacuumizes, and the material mixed is sucked hydrogenation still; Hydrogenation still is replaced, is replaced rear increase still internal pressure to 12kg/cm
2, start magnetic stirring vessel and stir, in hydrogenation process, regulate hydrogen valve, keep still internal pressure 12kg/cm
2; Keep temperature 50 C, stir 1 hour; Releasing hydrogen gas, replaces into nitrogen 10kg, opens and stirs cooling pan filtration; Hydrogenation still is replaced, makes binder and prepare; Feed liquid nitrogen pressure in hydrogenation still is slowly depressed in suction filtration bucket and carries out suction filtration; Filtrate sucks still kettle, and palladium charcoal is cleaned with DMF and reclaimed.
3) salify analysis of material workshop section
Add feed liquid suction still kettle, after exhausting, heat temperature raising carries out underpressure distillation, and distill when temperature in the kettle adds to 120 DEG C and terminate, underpressure distillation keeps vacuum tightness 0.085MPa, automatic steam control 0.1MPa; Open cooling water valve, temperature in the kettle is cooled to 45 DEG C; Open water rushes pump and vacuumizes still kettle, 1000kg water and 186kg hydrochloric acid is sucked still kettle, stirs 30 minutes; Close water and rush pump, add 60kg gac; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, keep temperature 89 DEG C, stir decolouring 1 hour; Decolouring terminates, and filter immediately, filtrate enters finished product still kettle, and gac turns over and washes once simultaneously, then is 3 with 70 DEG C of water rinses to pH value, and washing water water rushes pump and sucks still kettle; When still kettle stirring rake encounters filtrate, open underpressure distillation, rotating speed keeps 1450 rpms; When there being material to separate out in still, speed governing 1050 rpms, continues distillation 1 hour, then closes distillation, speed governing 600 rpms, and chuck enters tap water cooling, rotating speed 530 turns during cooling, and cooling pan not emptying during cooling keeps vacuum tightness; Temperature in the kettle is cooled to less than 35 DEG C, and chuck uses chilled brine instead, treats that temperature in the kettle is cooled to 0 DEG C, continues stirring 1 hour; Stir terminate whizzer need first with the hydrochloric acid water rinsing that the PH of 5kg is 1, blowing suction filtration, drain after divide three times centrifugal, centrifugal 1 hour at every turn; Suction filtration filtrate recovery, mark is carried out in centrifugal end, proceeds to drying section and finally obtains 2,4-diaminophenoxy ethanol hydrochloride, 2,4-diaminophenoxy ethanol hydrochloric acid salts contg≤99.37, yield 93%, the filtrate rate of recovery 92%.
Embodiment 3
Carry out production 2,4-diaminophenoxy ethanol hydrochloride
1) condensation workshop section
Open vacuum system, 400kg ethylene glycol is sucked in pot, then opens stirring, suck the 160kg2 dissolved in advance, after 4-dinitrochlorobenzene, again suck 200kg ethylene glycol, keep temperature 80 DEG C; Open manhole, dropped in still by 45kg sodium carbonate, build manhole, open emptying valve, open water rushes pump and vacuumizes in still; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, after water of condensation all drains, then switch to trap; Keep temperature 140 DEG C, pH value 8, closes water after draining carbonic acid gas and rushes pump, stirs 6 hours; Insulation reaction terminates, sampling be TLC analyze qualified after, add 1000kg water, be warming up to 95 DEG C, stir 2 hours; Leave standstill 30 minutes, then supernatant liquid is sucked continuation cooling in cooling reactor, when temperature in the kettle is down to 40 DEG C, switch chilled brine, continue to be cooled to 20 DEG C, blowing suction filtration, obtain condensation material 165kg; Suction filtration terminates, and filter cake to neutral, divides secondary centrifuging with ionized water rinsing, centrifugal 1 hour at every turn, filtrate suction was reclaimed in pot, and centrifugal end is weighed, the standing lower floor's by product obtained for 30 minutes, after supernatant liquid sucks, adds mother liquor and is warming up to 90 DEG C, stir 15 minutes, blowing suction filtration, filtrate sucks cooling reactor and is cooled to 15 DEG C, filter residue rinsed clean, and filter residue rinsing pH value keeps 7, barrelling after centrifuge dripping, and carry out mark.
2) hydrogenating reduction workshop section
165kg condensation material is added 560kgDMF and 2.7kg palladium charcoal, mixing and stirring; Hydrogenation still vacuumizes, and the material mixed is sucked hydrogenation still; Hydrogenation still is replaced, is replaced rear increase still internal pressure to 12kg/cm
2, start magnetic stirring vessel and stir, in hydrogenation process, regulate hydrogen valve, keep still internal pressure 12kg/cm
2; Keep temperature 60 C, stir 1 hour; Releasing hydrogen gas, replaces into nitrogen 10kg, opens and stirs cooling pan filtration; Hydrogenation still is replaced, makes binder and prepare; Feed liquid nitrogen pressure in hydrogenation still is slowly depressed in suction filtration bucket and carries out suction filtration; Filtrate sucks still kettle, and palladium charcoal is cleaned with DMF and reclaimed.
3) salify analysis of material workshop section
Add feed liquid suction still kettle, after exhausting, heat temperature raising carries out underpressure distillation, and distill when temperature in the kettle adds to 120 DEG C and terminate, underpressure distillation keeps vacuum tightness 0.085MPa, automatic steam control 0.1MPa; Open cooling water valve, temperature in the kettle is cooled to 50 DEG C; Open water rushes pump and vacuumizes still kettle, 1000kg water and 186kg hydrochloric acid is sucked still kettle, stirs 30 minutes; Close water and rush pump, add 60kg gac; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, keep temperature 90 DEG C, stir decolouring 1 hour; Decolouring terminates, and filter immediately, filtrate enters finished product still kettle, and gac turns over and washes once simultaneously, then is 4 with 80 DEG C of water rinses to pH value, and washing water water rushes pump and sucks still kettle; When still kettle stirring rake encounters filtrate, open underpressure distillation, rotating speed keeps 1450 rpms; When there being material to separate out in still, speed governing 1050 rpms, continues distillation 1 hour, then closes distillation, speed governing 600 rpms, and chuck enters tap water cooling, rotating speed 530 turns during cooling, and cooling pan not emptying during cooling keeps vacuum tightness; Temperature in the kettle is cooled to less than 40 DEG C, and chuck uses chilled brine instead, treats that temperature in the kettle is cooled to 0 DEG C, continues stirring 2 hours; Stir terminate whizzer need first with the hydrochloric acid water rinsing that the PH of 5kg is 1, blowing suction filtration, drain after divide three times centrifugal, centrifugal 1 hour at every turn; Suction filtration filtrate recovery, mark is carried out in centrifugal end, proceeds to drying section and finally obtains 2,4-diaminophenoxy ethanol hydrochloride, 2,4-diaminophenoxy ethanol hydrochloric acid salts contg≤99.27, yield 92%, the filtrate rate of recovery 91%.
Claims (7)
1. the manufacturing process of a diaminophenoxy ethanol hydrochloride, is characterized in that: comprise the following steps:
1) condensation workshop section
Open vacuum system, ethylene glycol is sucked in pot, then open stirring, after sucking the DNFB dissolved in advance, again suck ethylene glycol, keep temperature 60 ~ 80 DEG C; Open manhole, dropped into by sodium carbonate in still, build manhole, open emptying valve, open water rushes pump and vacuumizes in still; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, after water of condensation all drains, then switch to trap; Keep temperature 100 ~ 140 DEG C, pH value 7.5 ~ 8, closes water after draining carbonic acid gas and rushes pump, stirs 4 ~ 6 hours; Insulation reaction terminates, sampling be TLC analyze qualified after, add 1000kg water, be warming up to 90 ~ 95 DEG C, stir 1 hour; Leave standstill 30 minutes, then supernatant liquid is sucked continuation cooling in cooling reactor, when temperature in the kettle is down to 30 ~ 40 DEG C, switch chilled brine, continue to be cooled to 10 ~ 20 DEG C, blowing suction filtration, obtain condensation material; Suction filtration terminates, and filter cake is with ionized water rinsing to neutral, and divide secondary centrifuging, centrifugal 1 ~ 2 hour at every turn, filtrate suction is reclaimed in pot, and centrifugal end is weighed;
2) hydrogenating reduction workshop section
Condensation material is added DMF and palladium charcoal, mixing and stirring; Hydrogenation still vacuumizes, and the material mixed is sucked hydrogenation still; Hydrogenation still is replaced, is replaced rear increase still internal pressure to 12kg/cm
2, start magnetic stirring vessel and stir; Keep temperature 40 ~ 60 DEG C, stir 1 ~ 2 hour; Releasing hydrogen gas, replaces into nitrogen 10kg, opens and stirs cooling pan filtration; Hydrogenation still is replaced, makes binder and prepare; Feed liquid nitrogen pressure in hydrogenation still is slowly depressed in suction filtration bucket and carries out suction filtration; Filtrate sucks still kettle, and palladium charcoal is cleaned with DMF and reclaimed;
3) salify analysis of material workshop section
Add feed liquid suction still kettle, after exhausting, heat temperature raising carries out underpressure distillation, distills and terminate when temperature in the kettle adds to 120 DEG C; Open cooling water valve, temperature in the kettle is cooled to 40 ~ 50 DEG C; Open water rushes pump and vacuumizes still kettle, water and hydrochloric acid is sucked still kettle, stirs 30 minutes; Close water and rush pump, add gac; Open jacket steam valve, then open the bypath valve of trap, lead pouring draining, keep temperature 88 ~ 90 DEG C, stir decolouring 1 hour; Decolouring terminates, and filter immediately, filtrate enters finished product still kettle, and gac turns over and washes once simultaneously, then uses 60 ~ 80 DEG C of water rinses to pH value 3 ~ 4, and washing water water rushes pump and sucks still kettle; When still kettle stirring rake encounters filtrate, open underpressure distillation, rotating speed keeps 1450 rpms; When there being material to separate out in still, speed governing 1050 rpms, continues distillation 1 hour, then closes distillation, speed governing 600 rpms, and chuck enters tap water cooling, rotating speed 530 turns during cooling; Temperature in the kettle is cooled to less than 30 ~ 40 DEG C, and chuck uses chilled brine instead, treats that temperature in the kettle is cooled to 0 DEG C, continues stirring 1 hour; Stir and terminate blowing suction filtration, after draining points three times centrifugal, centrifugal 1 ~ 2 hour at every turn; Suction filtration filtrate recovery, mark is carried out in centrifugal end, proceeds to drying section and finally obtains 2,4-diaminophenoxy ethanol hydrochloride.
2. according to claim 12, the manufacturing process of 4-diaminophenoxy ethanol hydrochloride, it is characterized in that: the lower floor's by product obtained after described condensation workshop section leaves standstill 30 minutes is after supernatant liquid sucks, add mother liquor and be warming up to 90 DEG C, stir 15 minutes, blowing suction filtration, filtrate sucks cooling reactor and is cooled to 15 DEG C, filter residue rinsed clean, barrelling after centrifuge dripping, and carry out mark.
3. the manufacturing process of 2,4-diaminophenoxy ethanol hydrochlorides according to claim 1, is characterized in that: in described hydrogenating reduction workshop section hydrogenation process, regulates hydrogen valve, keeps still internal pressure 12kg/cm
2.
4. the manufacturing process of 2,4-diaminophenoxy ethanol hydrochlorides according to claim 1, is characterized in that: the underpressure distillation of described salify analysis of material workshop section keeps vacuum tightness 0.085MPa, automatic steam control 0.1MPa.
5. the manufacturing process of 2,4-diaminophenoxy ethanol hydrochlorides according to claim 1, is characterized in that: cooling pan not emptying during described salify analysis of material workshop section cooling, keeps vacuum tightness.
6. the manufacturing process of 2,4-diaminophenoxy ethanol hydrochlorides according to claim 1, is characterized in that: described salify analysis of material workshop section whizzer need first with the hydrochloric acid water rinsing that the PH of 5kg is 1.
7. the manufacturing process of 2,4-diaminophenoxy ethanol hydrochlorides according to claim 2, is characterized in that: described condensation workshop section filter residue rinsing pH value keeps 7 ~ 7.5.
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| CN106397212A (en) * | 2016-09-14 | 2017-02-15 | 重庆市碚圣医药科技股份有限公司 | Method for preparation of 2, 4-dinitrophenoxyethanol |
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| Pd- Fe 吸附树脂催化合成β- ( 2, 4- 二氨基苯氧基) 乙醇盐酸盐;蔡照胜 等;《现代化工》;20070630;第27卷;第216-219页 * |
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