CN108752222A - A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers - Google Patents
A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers Download PDFInfo
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- CN108752222A CN108752222A CN201810950496.7A CN201810950496A CN108752222A CN 108752222 A CN108752222 A CN 108752222A CN 201810950496 A CN201810950496 A CN 201810950496A CN 108752222 A CN108752222 A CN 108752222A
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- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
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Abstract
The present invention relates to the purification technique fields of fine chemistry industry organic material, especially the crystallization and purification technique and crystallization and purification system of one kind 4,4'- diaminodiphenyl ethers.The crystallization and purification technique and crystallization and purification system of one kind 4,4'- diaminodiphenyl ethers of the present invention, method is simple and quick, and purification system is practical and convenient；Make 4,4'- diaminodiphenyl ethers purity up to 99.8% or more after purification, reaches as high as 99.93%；It is 0.5-1L/min by control loop water flow, adjusting crystallization kettle speed of agitator is 40-60r/min, makes final product grain size in 1mm or less；Cycling and reutilization after purification solvent is recyclable, economizes on resources；4,4'- diaminodiphenyl ethers after the present invention purifies fully meet the demand that domestic and international market produces high-end product.
Description
Technical field
The present invention relates to the purification technique fields of fine chemistry industry organic material, especially one kind 4,4'- diaminodiphenyl ethers
Crystallization and purification technique and crystallization and purification system.
Background technology
4,4 '-diaminodiphenyl ether English names：4,4'-dimido diphenylaether, abbreviation ODA.ODA is one
The important high polymer monomer of kind, the polyimide resin synthesized by it, polymaleimide resins, one imide resin of polyamide
It is widely used in some new and high technologies, this resinoid performance most outstanding is high temperature resistant, can be used continuously at 260 DEG C,
Interval temperature in use is up to 480 DEG C.With good insulating properties, higher intensity, wearability and chemical stability outstanding are excellent
Good lubricity and shielding property.Molded product, glass fiber reinforced layer, film and electric wire paint etc. are can be made into, it is main to apply
It insulate in the inside and outside layer of aircraft, rocket heat proof cable, the layer insulation of transformer, the liner etc. of motor.Using this resinoid
Afterwards, small design can be made.4,4'- diaminodiphenyl ethers are synthesis 3,3 ' 4, the raw material of 4 '-tetramino diphenyl ether, Hou Zheshi
Produce the principal monomer of the heat-resisting heterocyclic polymer of a series of new such as polybenzimidazoles, polyphenylene quinoline, polyimidazole pyridine.Also may be used
Crosslinking agent as high-molecular compounds such as heat-resistance epoxy resin, polyurethanes.
The synthesis of ODA：The synthetic population of ODA in two steps, first, 4,4 '-dinitro diphenyl ether (English names:4,4-
Dinitrodiphenylether abbreviation DNDPE) synthesis, another step be by DNDPE through reduction obtain 4,4 '-diamino two
Phenylate.DNDPE is typically a kind of crystalline solid particle of yellow, and chemical property is stablized, by paranitrophenol sodium salt (potassium) and to chlorine
Nitrobenzene is condensed.The method is traditional industrializing synthesis route, and paranitrophenol sodium salt (potassium) then can directly and parachloronitrobenzene
Condensation.Select solvent and catalyst appropriate that can be conducive to improve mass transfer effect, to reduce reaction temperature, shorten the reaction time.
Common solvent has nitrobenzene, DMF, DMSO etc..Common catalyst has potassium chloride, sodium carbonate (potassium), yield 90% with
On.
The synthetic method of ODA：ODA is white crystal, relative density 1.315,300 DEG C of boiling point or more, fusing point 191.5
DEG C, 219 DEG C of ignition point, 490 DEG C of ignition point.It is soluble in dilute hydrochloric acid, it is not soluble in water.The commercial synthesis of ODA is all to use
DNDPE is raw material, is made through reduction.
Hydrogen reduction：Hydrogen reduction is the advanced technologies used both at home and abroad, at low cost, high income, product
The advantages that high-quality.Corresponding appropriate solvent is selected, under a certain pressure, obtains ODA through one carbon catalytic hydrogenation of palladium, then through rising
China and obtain finished product.
4, the 4'- diaminodiphenyl ethers produced by process above, are irregular big bulks, and product quality is uneven
Even, purity is low, and purity only has 99.5%, cannot meet the needs of domestic and international market client produces high-end product.
Invention content
The purpose of the present invention is to provide a kind of crystallization and purification technique of 4,4'- diaminodiphenyl ethers and crystallization and purification systems
System, overcomes aforementioned 4, the 4'- diaminodiphenyl ether product qualities produced in the prior art uneven, the low deficiency of purity,
Make 4,4'- diaminodiphenyl ethers purity up to 99.8% or more after purification, grain size in 1mm hereinafter, and purification with solvent it is recyclable after follow
Ring recycles.
The technical scheme adopted by the invention to solve the technical problem is that：
The crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers, including following operating procedure：
（1）Check crystallization kettle, it is ensured that each junction of crystallization kettle is without gas leak phenomenon, it is ensured that crystallization kettle recirculated water is unimpeded, it is ensured that knot
Brilliant kettle machine seal pressure is not less than 0.95Mpa；
（2）Solvent pump is opened, is squeezed into solvent in measuring tank by solvent pump, after closing solvent pump, by measuring tank by solvent
It is put into crystallization kettle；
（3）The quality and quantity of crystallization kettle internal solvent are observed using illuminations, opens frequency modulator, and frequency modulation control is opened in 15Hz
Begin to launch irregular blocky thick 4,4'- diaminodiphenyl ethers;
（4）Step（3）It after the completion of feeding intake, is replaced 3 times with nitrogen, closed crystallization kettle, to prevent thick 4, the 4'- of irregular bulk bis-
Amino-diphenylethers is aoxidized；
（5）Lead to steam to crystallization kettle chuck, be heated to 100-130 DEG C, until pressure is 0.75Mpa, crystallization kettle in crystallization kettle
When jacket steam pressure is 0.4Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 0.5-2h；
（6）After the completion of heat preservation, start to be passed through circulating water cooling in crystallization kettle chuck, control loop water flow is 0.5-1L/
Min, adjusting crystallization kettle speed of agitator are 40-60r/min；
（7）When being cooled to 20-40 DEG C, the bottom valve of crystallization kettle is opened, the material in crystallization kettle is put and is filtered into suction filtration tank；
（8）Step（7）It filters obtained crystalline mother solution to put to distilling in distillation still, recycling design recycles, and vapo(u)rizing temperature is
65-68 DEG C, distillation duration 3-4h；
（9）Step（7）In the filter cake input vacuum drier obtained after suction filtration, temperature control at 90-92 DEG C, vacuum degree≤-
0.08Mpa, dry 1-3h is to get finished product 4,4'- diaminodiphenyl ethers.
Preferably, the step（2）In solvent be methanol, ethyl alcohol, to ethylo benzene methyl ether, dimethylformamide, diformazan
One kind in yl acetamide.
Preferably, the step（2）In solvent be methanol.
Preferably, the step（2）The weight and step of middle solvent（3）In irregular blocky thick 4,4'- diamino two
The weight ratio of phenylate is 3-5:1.
Preferably, the step（2）The weight and step of middle solvent（3）In irregular blocky thick 4,4'- diamino two
The weight ratio of phenylate is 4:1.
Preferably, the step（5）In, lead to steam to crystallization kettle chuck, 117 DEG C is heated to, until crystallization kettle internal pressure
When power is 0.75Mpa, crystallization kettle jacket steam pressure is 0.4Mpa, steam off switch, the kettle temperature of crystallization kettle rises to 126 DEG C,
Keep the temperature 1h.
Preferably, the step（6）In, control loop water flow is 0.8L/min, adjusts crystallization kettle speed of agitator and is
50r/min。
Preferably, the step（8）In, when distillation a length of 3.5h.
Preferably, the step（9）In, drying time 2h.
The crystallization and purification system of one kind 4,4'- diaminodiphenyl ethers, including crystallization kettle, connect with crystallization kettle measuring tank,
The suction filtration tank being connect with crystallization kettle, the distillation still being connect with suction filtration tank and the vacuum desiccator being connect with suction filtration tank.
The beneficial effects of the invention are as follows：Compared with prior art, the crystallization of one kind 4,4'- diaminodiphenyl ethers of the invention
Purifying technique and crystallization and purification system, method is simple and quick, and purification system is practical and convenient；Make 4,4'- diamino hexichol after purification
Ether purity reaches as high as 99.93% up to 99.8% or more；It is 0.5-1L/min by control loop water flow, adjusts crystallization kettle and stir
Mix rotating speed is 40-60r/min, makes final product grain size in 1mm or less；Cycling and reutilization after purification solvent is recyclable is saved
Resource；4,4'- diaminodiphenyl ethers after the present invention purifies fully meet the demand that domestic and international market produces high-end product.
Description of the drawings
Fig. 1 is a kind of crystallization and purification system structure diagram of 4,4'- diaminodiphenyl ethers of the embodiment of the present invention 4；
Wherein, 1 crystallization kettle, 2 measuring tanks, 3 suction filtration tanks, 4 distillation stills, 5 vacuum desiccators, 6 first pipelines, 7 second pipelines, 8
Three pipelines, 9 crude product batch feeding ends, 10 finished product discharge ends.
Specific implementation mode
A kind of crystallization and purification technique of 1 4,4'- diaminodiphenyl ethers of embodiment
The crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers, including following operating procedure：
（1）Check crystallization kettle, it is ensured that each junction of crystallization kettle is without gas leak phenomenon, it is ensured that crystallization kettle recirculated water is unimpeded, it is ensured that knot
Brilliant kettle machine seal pressure is not less than 0.95Mpa；
（2）Solvent pump is opened, is squeezed into 1200kg solvent methanols in measuring tank by solvent pump, after closing solvent pump, passes through meter
Solvent methanol is put into crystallization kettle by measuring tank；
（3）The quality and quantity of crystallization kettle internal solvent are observed using illuminations, opens frequency modulator, and frequency modulation control is opened in 15Hz
Begin to launch thick 4, the 4'- diaminodiphenyl ethers of irregular bulk that purity is 99.5%, launches 300kg altogether；
（4）Step（3）It after the completion of feeding intake, is replaced 3 times with nitrogen, closed crystallization kettle, to prevent thick 4, the 4'- of irregular bulk bis-
Amino-diphenylethers is aoxidized；
（5）Lead to steam to crystallization kettle chuck, be heated to 117 DEG C, until pressure is 0.75Mpa, crystallization kettle chuck in crystallization kettle
When steam pressure is 0.4Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 1h；
（6）After the completion of heat preservation, starting to be passed through circulating water cooling in crystallization kettle chuck, control loop water flow is 0.8L/min,
Adjusting crystallization kettle speed of agitator is 50r/min；
（7）When being cooled to 30 DEG C, the bottom valve of crystallization kettle is opened, the material in crystallization kettle is put and is filtered into suction filtration tank；
（8）Step（7）It filters obtained crystalline mother solution to put to distilling in distillation still, recycling design recycles, and vapo(u)rizing temperature is
65-68 DEG C, distillation duration 3.5h；
（9）Step（7）In the filter cake input vacuum drier obtained after suction filtration, temperature control at 90-92 DEG C, vacuum degree≤-
0.08Mpa, dry 2h is to get finished product 4,4'- diaminodiphenyl ethers.
In the present embodiment, the crystallization kettle used is enamel material, and crystallization kettle volume is 2m3.
A kind of crystallization and purification technique of 2 4,4'- diaminodiphenyl ethers of embodiment
The crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers, including following operating procedure：
（1）Check crystallization kettle, it is ensured that each junction of crystallization kettle is without gas leak phenomenon, it is ensured that crystallization kettle recirculated water is unimpeded, it is ensured that knot
Brilliant kettle machine seal pressure is not less than 0.95Mpa；
（2）Solvent pump is opened, is squeezed into 1200kg solvent methanols in measuring tank by solvent pump, after closing solvent pump, passes through meter
Solvent methanol is put into crystallization kettle by measuring tank；
（3）The quality and quantity of crystallization kettle internal solvent are observed using illuminations, opens frequency modulator, and frequency modulation control is opened in 15Hz
Begin to launch thick 4, the 4'- diaminodiphenyl ethers of irregular bulk that purity is 99.5%, launches 240kg altogether；
（4）Step（3）It after the completion of feeding intake, is replaced 3 times with nitrogen, closed crystallization kettle, to prevent thick 4, the 4'- of irregular bulk bis-
Amino-diphenylethers is aoxidized；
（5）Lead to steam to crystallization kettle chuck, be heated to 110 DEG C, until pressure is 0.75Mpa, crystallization kettle chuck in crystallization kettle
When steam pressure is 0.4Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 0.8h；
（6）After the completion of heat preservation, starting to be passed through circulating water cooling in crystallization kettle chuck, control loop water flow is 0.6L/min,
Adjusting crystallization kettle speed of agitator is 40r/min；
（7）When being cooled to 30 DEG C, the bottom valve of crystallization kettle is opened, the material in crystallization kettle is put and is filtered into suction filtration tank；
（8）Step（7）It filters obtained crystalline mother solution to put to distilling in distillation still, recycling design recycles, and vapo(u)rizing temperature is
65-68 DEG C, distillation duration 3h；
（9）Step（7）In the filter cake input vacuum drier obtained after suction filtration, temperature control at 90-92 DEG C, vacuum degree≤-
0.08Mpa, dry 1.5h is to get finished product 4,4'- diaminodiphenyl ethers.
In the present embodiment, the crystallization kettle used is enamel material, and crystallization kettle volume is 2m3.
A kind of crystallization and purification technique of 3 4,4'- diaminodiphenyl ethers of embodiment
The crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers, including following operating procedure：
（1）Check crystallization kettle, it is ensured that each junction of crystallization kettle is without gas leak phenomenon, it is ensured that crystallization kettle recirculated water is unimpeded, it is ensured that knot
Brilliant kettle machine seal pressure is not less than 0.95Mpa；
（2）Solvent pump is opened, is squeezed into 1200kg solvent methanols in measuring tank by solvent pump, after closing solvent pump, passes through meter
Solvent methanol is put into crystallization kettle by measuring tank；
（3）The quality and quantity of crystallization kettle internal solvent are observed using illuminations, opens frequency modulator, and frequency modulation control is opened in 15Hz
Begin to launch thick 4, the 4'- diaminodiphenyl ethers of irregular bulk that purity is 99.5%, launches 400kg altogether；
（4）Step（3）It after the completion of feeding intake, is replaced 3 times with nitrogen, closed crystallization kettle, to prevent thick 4, the 4'- of irregular bulk bis-
Amino-diphenylethers is aoxidized；
（5）Lead to steam to crystallization kettle chuck, be heated to 125 DEG C, until pressure is 0.75Mpa, crystallization kettle chuck in crystallization kettle
When steam pressure is 0.4Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 2h；
（6）After the completion of heat preservation, start to be passed through circulating water cooling in crystallization kettle chuck, control loop water flow is 1L/min, is adjusted
Section crystallization kettle speed of agitator is 60r/min；
（7）When being cooled to 30 DEG C, the bottom valve of crystallization kettle is opened, the material in crystallization kettle is put and is filtered into suction filtration tank；
（8）Step（7）It filters obtained crystalline mother solution to put to distilling in distillation still, recycling design recycles, and vapo(u)rizing temperature is
65-68 DEG C, distillation duration 4h；
（9）Step（7）In the filter cake input vacuum drier obtained after suction filtration, temperature control at 90-92 DEG C, vacuum degree≤-
0.08Mpa, dry 3h is to get finished product 4,4'- diaminodiphenyl ethers.
In the present embodiment, the crystallization kettle used is enamel material, and crystallization kettle volume is 2m3.
A kind of crystallization and purification system of 4 4,4'- diaminodiphenyl ethers of embodiment
As shown in Figure 1, the crystallization and purification system of one kind 4,4'- diaminodiphenyl ethers, including crystallization kettle 1, it is connect with crystallization kettle 1
Measuring tank 2, the suction filtration tank 3 being connect with crystallization kettle 1, the distillation still 4 being connect with suction filtration tank 3 and the vacuum being connect with suction filtration tank 3 are dry
Dry device 5.Material in crystallization kettle 1 enters suction filtration tank 3 by the first pipeline 6, and 3 filtered crystalline mother solution of suction filtration tank passes through second
Pipeline 7 enters distillation still 4,3 filtered filter cake of suction filtration tank（Crystallize wet 4,4'- diaminodiphenyl ethers）Pass through third pipeline 8
Into vacuum desiccator 5.Irregular thick 4, the 4'- diaminodiphenyl ethers of bulk enter from crude product batch feeding end 9, finished product 4,4'- bis-
Amino-diphenylethers is released from finished product discharge end 10.
The operation principle of the present embodiment is shown in a kind of crystallization and purification technique of 4,4'- diaminodiphenyl ethers in embodiment 1-3
Concrete operation step.
The measurement of 1 4,4'- diaminodiphenyl ether product contents of experimental example
Experimental method：After 4, the 4'- diaminodiphenyl ethers of gained after embodiment 1-3 crystallization and purifications are dissolved in a solvent, utilize
Gas-chromatography makes 4,4 '-diaminodiphenyl ethers and other components be detached in corresponding pillar, is put by hydrogen flame micro-current
Big device amplifies and records chromatogram by chromatographic work station, to obtain the content of 4,4 '-diaminodiphenyl ethers and other components.
Experiment material：Nitrogen：Purity is more than 99.99%；Hydrogen：Purity is more than 99.99%；Air：It is filled through molecular sieve, silica gel
Divide dry and purification；Solvent：Dimethylformamide（It analyzes pure）.
Instrument and equipment：Gas chromatograph：Instrumental sensitivity should meet the regulation of GB9722 with stability；Detector：Hydrogen
Flame ionization detector；Injector：1uL micro syringes；Chromatographic column：Fixer：HP-5, wide bore capillary column, internal diameter：
0.45mm, it is long：30m.
Gas chromatograph operating condition：Column compartment temperature：180-220 DEG C or temperature appropriate is selected by user；Sample introduction temperature
Degree：250-280℃；Detect temperature：250-280℃；Carrier gas（Nitrogen）Flow：4ml/min；Hydrogen:Flow：20ml/min；It is empty
Gas：400-700ml/min；Septum purge：2ml/min；Shunting：40ml/min；Sample size：0.5uL.
Determination step：Points 3 groups weigh the 4,4 '-each 0.3g of diaminodiphenyl ether sample purified in embodiment 1-3 in 3 not
In same 10mL volumetric flasks,（It is accurate to 0.0001g）Add 10ml solvents, shake up, after placing dissolving, under given conditions, uses
1uL microsyringes are drawn in 0.5uL sample solutions injection chromatography and are analyzed, and automatic printing is gone out result by chromatographic work station.
To same sample, its analysis result is indicated with the arithmetic mean of instantaneous value of measurement result twice.
Test structure is as shown in table 1：
Table 1
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| 4,4 '-diaminodiphenyl ether purity（%） | 99.93% | 99.87% | 99.81% |
As can be seen from Table 1,4,4'- after the crystallization and purification technique purification of one kind 4,4'- diaminodiphenyl ethers through the present invention
Diaminodiphenyl ether, purity are highly improved, and are that 99.5% to be promoted to purity be 99.8% or more by original purity, especially
It is 4, the 4'- diaminodiphenyl ethers purified in the embodiment of the present invention 1, purity is up to 99.93%, fully meets domestic and international city
The demand of field production high-end product.In addition, used in the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers of the present invention
Solvent can recycle cycling and reutilization after distillation still is distilled, and economize on resources.
2 4,4'- diaminodiphenyl ether granule detecting methods of experimental example
Laboratory apparatus：The stainless steel standard of 1mm is sieved.
Experimental Procedures Procedure：Divide 3 100 grams of crystallization 4,4'- diamino hexichol weighed respectively after being purified in embodiment 1-3
Ether sample pours into the standard screen Inside sifter of 1mm respectively, and the part mass for weighing sieving is M grams, granularity=M/100 × 100%,
Granularity is more than 95% for qualification.
Experimental result is as shown in table 2：
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| 4,4 '-diaminodiphenyl ether granularities（%） | 99.99% | 99.98% | 99.99% |
There is table 2 to can be seen that 4,4'- after the crystallization and purification technique purification of one kind 4,4'- diaminodiphenyl ethers through the present invention
Diaminodiphenyl ether, grain size are less than 1mm, uniform in quality.
Above-mentioned specific implementation mode is only the specific case of the present invention, and scope of patent protection of the invention includes but not limited to
The product form and style of above-mentioned specific implementation mode, any claims of the present invention and any technical field of meeting
The appropriate changes or modifications that those of ordinary skill does it, all shall fall within the protection scope of the present invention.
Claims (10)
1. one kind 4, the crystallization and purification technique of 4'- diaminodiphenyl ethers, it is characterised in that：Including following operating procedure：
（1）Check crystallization kettle, it is ensured that each junction of crystallization kettle is without gas leak phenomenon, it is ensured that crystallization kettle recirculated water is unimpeded, it is ensured that knot
Brilliant kettle machine seal pressure is not less than 0.95Mpa；
（2）Solvent pump is opened, is squeezed into solvent in measuring tank by solvent pump, after closing solvent pump, by measuring tank by solvent
It is put into crystallization kettle；
（3）The quality and quantity of crystallization kettle internal solvent are observed using illuminations, opens frequency modulator, and frequency modulation control is opened in 15Hz
Begin to launch irregular blocky thick 4,4'- diaminodiphenyl ethers;
（4）Step（3）It after the completion of feeding intake, is replaced 3 times with nitrogen, closed crystallization kettle, to prevent thick 4, the 4'- of irregular bulk bis-
Amino-diphenylethers is aoxidized；
（5）Lead to steam to crystallization kettle chuck, be heated to 100-130 DEG C, until pressure is 0.75Mpa, crystallization kettle in crystallization kettle
When jacket steam pressure is 0.4Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 0.5-2h；
（6）After the completion of heat preservation, start to be passed through circulating water cooling in crystallization kettle chuck, control loop water flow is 0.5-1L/
Min, adjusting crystallization kettle speed of agitator are 40-60r/min；
（7）When being cooled to 20-40 DEG C, the bottom valve of crystallization kettle is opened, the material in crystallization kettle is put and is filtered into suction filtration tank；
（8）Step（7）It filters obtained crystalline mother solution to put to distilling in distillation still, recycling design recycles, and vapo(u)rizing temperature is
65-68 DEG C, distillation duration 3-4h；
（9）Step（7）In the filter cake input vacuum drier obtained after suction filtration, temperature control at 90-92 DEG C, vacuum degree≤-
0.08Mpa, dry 1-3h is to get finished product 4,4'- diaminodiphenyl ethers.
2. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（2）In solvent be methanol, ethyl alcohol, to one kind in ethylo benzene methyl ether, dimethylformamide, dimethylacetylamide.
3. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as claimed in claim 2, it is characterised in that：The step
Suddenly（2）In solvent be methanol.
4. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（2）The weight and step of middle solvent（3）In the weight ratios of irregular blocky thick 4,4'- diaminodiphenyl ethers be 3-5:1.
5. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（2）The weight and step of middle solvent（3）In the weight ratios of irregular blocky thick 4,4'- diaminodiphenyl ethers be 4:1.
6. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（5）In, lead to steam to crystallization kettle chuck, be heated to 117 DEG C, until pressure is 0.75Mpa, crystallization kettle chuck in crystallization kettle
When steam pressure is 0.55Mpa, the kettle temperature of steam off switch, crystallization kettle rises to 126 DEG C, keeps the temperature 1h.
7. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（6）In, control loop water flow is 0.8L/min, and adjusting crystallization kettle speed of agitator is 50r/min.
8. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（8）In, when distillation a length of 3.5h.
9. the crystallization and purification technique of one kind 4,4'- diaminodiphenyl ethers as described in claim 1, it is characterised in that：The step
Suddenly（9）In, drying time 2h.
10. one kind 4, the crystallization and purification system of 4'- diaminodiphenyl ethers, it is characterised in that：It is connect including crystallization kettle, with crystallization kettle
Measuring tank, the suction filtration tank being connect with crystallization kettle, the distillation still being connect with suction filtration tank and the vacuum desiccator being connect with suction filtration tank.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110015965A (en) * | 2019-04-26 | 2019-07-16 | 山东欧亚化工有限公司 | A method of 4,4 '-diaminodiphenyl ether secondary crystallizations of production |
| CN115010612A (en) * | 2022-06-24 | 2022-09-06 | 河北海力香料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
| CN117030919A (en) * | 2023-10-09 | 2023-11-10 | 山东欧亚高分子材料有限公司 | Gas chromatography detection method for 4,4' -diaminodiphenyl ether content |
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| CN107162919A (en) * | 2017-07-13 | 2017-09-15 | 山东冠森高分子材料科技股份有限公司 | Energy-efficient, environmentally friendly novel diamino diphenyl ether production line |
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| CN107162919A (en) * | 2017-07-13 | 2017-09-15 | 山东冠森高分子材料科技股份有限公司 | Energy-efficient, environmentally friendly novel diamino diphenyl ether production line |
| CN107353214A (en) * | 2017-07-13 | 2017-11-17 | 山东冠森高分子材料科技股份有限公司 | With the directly refined 4,4 ＇ diaminodiphenyl ether techniques of mixed solvent recrystallization |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110015965A (en) * | 2019-04-26 | 2019-07-16 | 山东欧亚化工有限公司 | A method of 4,4 '-diaminodiphenyl ether secondary crystallizations of production |
| CN115010612A (en) * | 2022-06-24 | 2022-09-06 | 河北海力香料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
| CN115010612B (en) * | 2022-06-24 | 2023-08-15 | 河北海力恒远新材料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
| CN117030919A (en) * | 2023-10-09 | 2023-11-10 | 山东欧亚高分子材料有限公司 | Gas chromatography detection method for 4,4' -diaminodiphenyl ether content |
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