CN103664645B - The industrialized process for preparing of 1,8-diaminonaphthalene - Google Patents
The industrialized process for preparing of 1,8-diaminonaphthalene Download PDFInfo
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- CN103664645B CN103664645B CN201310729848.3A CN201310729848A CN103664645B CN 103664645 B CN103664645 B CN 103664645B CN 201310729848 A CN201310729848 A CN 201310729848A CN 103664645 B CN103664645 B CN 103664645B
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Abstract
The invention discloses a kind of 1, the industrialized process for preparing of 8-diaminonaphthalene, catalyzer, dinitronaphthalene and solvent is added successively in reactor, material in still is made to be warming up to 65 DEG C ~ 75 DEG C under whipped state, slow dropping hydrazine hydrate, dropwise and continue to be warming up to 75 DEG C ~ 90 DEG C to material in reactor, be incubated 3 ~ 8 hours, terminate reaction; Press filtration after reacted material being cooled to 40 DEG C ~ 45 DEG C, carries out washing and recycling to the catalyzer that press filtration obtains, and washings and filtered liquid merge as feed liquid process; Feed liquid carries out decompression precipitation recycling design; In the feed liquid after precipitation, add 50 DEG C ~ 80 DEG C hot water carry out washing layering, upper strata is aqueous phase, and lower floor is feed liquid phase, and the feed liquid obtained by separatory sends into rectifying in rectifying tower mutually, and tower top obtains 1,8-diaminonaphthalene of purity >=99.5%.Can comprise water and organic solvent in dinitronaphthalene raw material, this organic solvent comprises organic solvent used when the nitrated after product of naphthalene carries out refining.
Description
Technical field
The present invention relates to the preparation method of 1,8-diaminonaphthalene, be specifically related to the industrialized process for preparing of 1,8-diaminonaphthalene.
Background technology
Diaminonaphthalene mainly comprises 1,5-diaminonaphthalene and 1,8-diaminonaphthalene, is important pigment intermediate; Wherein 1,8-diaminonaphthalene is the important intermediate manufacturing oil color, is mainly used in synthesis C.I. oil soluble orange 60# and oil soluble red 135 #.These two kinds of pigment are widely used in the painted of polystyrene, synthetic glass and rigid polyvinyl chloride and ABS.
Dinitronaphthalene reduction is the important channel of preparing diaminonaphthalene.The method that diaminonaphthalene is prepared in dinitronaphthalene reduction has iron powder reducing method, electrochemical reducing, catalytic hydrogenating reduction method and hydrazine hydrate reduction method etc.Although adopt that iron powder reducing legal system is gentle for diaminonaphthalene operational condition, technique is simple, side reaction is few, low for equipment requirements, three-waste pollution is serious and product yield is low, has started to be eliminated gradually.Electrochemical reducing has the advantages such as productive rate is high, easy and simple to handle, easily separated compared with iron powder reducing method, but the method energy consumption is high, only apply more at present in laboratory synthesis and half suitability for industrialized production, its high cost is not suitable for preparation of industrialization 1,8-diaminonaphthalene.Catalytic hydrogenating reduction legal system effectively can reduce three-waste pollution for diaminonaphthalene, has eco-friendly feature, but catalytic hydrogenating reduction method requires to use 1,8-refining dinitronaphthalene, otherwise can not get good effect, and refined material is more difficult; Equipment requirements is tight in addition, noble metal catalyst consumption is large, and cost is high.
Hydrazine hydrate reduction method reaction conditions is gentle, and the method processing ease, technique are simple, low to the requirement of material purity, are easy to realize industrialization.
Such as Chinese patent literature CN101823968B discloses a kind of hydrazine hydrate reduction 1,8-dinitronaphthalene prepares the method for 1,8-diaminonaphthalene, in the reactor of band stirrer reflux exchanger, add 1,8-dinitronaphthalene, catalyzer and polar organic solvent, open and stir, be warming up to 45 DEG C ~ 115 DEG C, in 1 ~ 3 hour, dripping concentration is the hydrazine hydrate of 40% ~ 80%, is incubated 3 ~ 8 hours, solution after must reacting; Solution filters after reacting, and reclaim catalyzer, filtrate Distillation recovery polar organic solvent, obtains feed liquid, toward feed liquid in, add cold water, and product is separated out, more after filtration, obtain 1,8-diaminonaphthalene after underpressure distillation; The mol ratio of described 1,8-dinitronaphthalene and hydrazine hydrate is 1: 3 ~ 4, and described catalyzer is 1: 2 ~ 10 to form by Iron trichloride hexahydrate and gac in mass ratio; Described organic solvent is the one in methyl alcohol, ethanol, Virahol, DMF.This method raw material used is 1,8-refining dinitronaphthalene, high to the requirement of reaction raw materials, does not give full play to the advantage of hydrazine hydrate reduction method; Due to the restriction of reaction raw materials, this method is not suitable for preparation of industrialization 1,8-diaminonaphthalene.This method is pure 1,8-dinitronaphthalene due to what adopt at present, is therefore situation about being made up of 1,8-dinitronaphthalene and 1,5-dinitronaphthalene for reaction raw materials, and how final product obtains 1,8-higher diaminonaphthalene of purity is the problem needing to solve.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of industrialized process for preparing of 1,8-diaminonaphthalene.
The technical scheme realizing the object of the invention is a kind of industrialized process for preparing of 1,8-diaminonaphthalene, comprises the following steps:
1. catalyzer, dinitronaphthalene and solvent is added successively to agitator, thermo detector, reflux exchanger, high-order dropping in the enamel reaction still of storage tank, then turn on agitator, material in still is made to be warming up to 65 DEG C ~ 75 DEG C under whipped state, the hydrazine hydrate of 80.1% ~ 100% is slowly dripped at such a temperature in 3 ~ 8 hours, hydrazine hydrate dropwises and continues to be warming up to 75 DEG C ~ 90 DEG C to material in reactor, be incubated 3 ~ 8 hours, terminate reaction; The mol ratio of dinitronaphthalene and hydrazine hydrate is 1: 3 ~ 4, and the quality of catalyzer is 2% ~ 10% of dinitronaphthalene quality, and the quality of solvent is 2 ~ 5 times of dinitronaphthalene quality.
2. press filtration after 1. reacted material is cooled to 40 DEG C ~ 45 DEG C by step, carry out washing and recycling to the catalyzer that press filtration obtains, washings and filtered liquid merge as feed liquid process.
3. the feed liquid 2. obtained step carries out decompression precipitation recycling design.
4. in the feed liquid after step 3. precipitation, add 50 DEG C ~ 80 DEG C hot water carry out washing layering, upper strata is aqueous phase, and lower floor is feed liquid phase, and the feed liquid obtained by separatory sends into rectifying in rectifying tower mutually, and tower top obtains 1,8-diaminonaphthalene of purity >=99.5%.
Above-mentioned steps 1. in solvent be methyl alcohol, ethanol or DMF; Or the mixed solvent that methyl alcohol, ethanol, DMF form with toluene respectively.
In the dinitronaphthalene that 1. above-mentioned steps adds in reactor, the purity of 1,8-dinitronaphthalene is more than or equal to 95%.
The dinitronaphthalene that 1. above-mentioned steps adds in reactor is damp product or dry product; Comprise water and organic solvent in described dinitronaphthalene tide product, organic solvent is methyl alcohol, ethanol, DMF or toluene.
Above-mentioned steps 1. in catalyzer be first ferric chloride hexahydrate is dissolved in water, gac is dispersed in alkaline aqueous solution and obtains suspension liquid; Then poured into by ferric chloride Solution in gac suspension liquid, the mass ratio of iron(ic) chloride and gac is 1: 2 ~ 5; After stirring, mixture filters, stand-by as catalyzer after filtering the filter cake oven dry obtained.
Above-mentioned steps is 2. after press filtration, and carry out washing and recycling with a small amount of methyl alcohol, ethanol or DMF to the catalyzer that press filtration obtains, washings and filtered liquid merge as feed liquid process.
Further, the step 3. solvent that obtains of feed liquid decompression precipitation is sent in rectifying tower and is processed, recycling design as step 1. in solvent use; During the solvent distillation that decompression precipitation obtains, the stage number of rectifying tower is 40 ~ 80, and feed liquid feeding temperature is 28 DEG C ~ 35 DEG C, and feed plate is 20th ~ 40 pieces; Trim the top of column ratio is 1: 4 ~ 10, and overhead condenser pressure is 0.098MPa ~ 1MPa; The solvent that tower top is recycled.
The present invention has positive effect: (1) preparation method of the present invention is to 1 in dinitronaphthalene raw material used, the purity requirement of 8-dinitronaphthalene is >=95%, and organic solvent and water can be comprised in dinitronaphthalene raw material, therefore can by nitrated for naphthalene obtain containing 1,5-dinitronaphthalene, 1, the damp product mixture of 8-dinitronaphthalene and other nitro-compound directly carries out refining removal major part 1,5-dinitronaphthalene, the refining rear damp product detecting 1,8-dinitronaphthalene purity >=95% in nitro compounds just can be used as the dinitronaphthalene raw material that preparation method of the present invention uses.
Because naphthalene is nitrated, refining after product without the need to drying, the preparation process of 1,8-dinitronaphthalene decreases dry link, saves the energy, avoids the danger that the long-term localized hyperthermia of nitro compounds causes simultaneously.
(2), during the hydrazine hydrate reduction of the industrialized process for preparing of 1,8-diaminonaphthalene of the present invention, the raw material dinitronaphthalene of use can be damp product or dry product; Described dinitronaphthalene tide product refer in dinitronaphthalene raw material and comprise water and organic solvent, and this organic solvent comprises organic solvent used when the nitrated after product of naphthalene carries out refining, concrete, and organic solvent is methyl alcohol, ethanol, DMF or toluene; The damp product of non-drying do not affect hydrazine hydrate reduction.
(3) the present invention is when carrying out reduction reaction, first take into account in the reactor of agitator drop into catalyzer, dinitronaphthalene and solvent to reflux exchanger, temperature, then after unlatching stirring carries out being warming up to 65 DEG C ~ 75 DEG C, slowly drip hydrazine hydrate at such a temperature, hydrazine hydrate dropwises and is slowly warming up to 75 DEG C ~ 90 DEG C to material in reactor, then insulation reaction afterwards.The present invention drips hydrazine hydrate after once temperature being risen to temperature of reaction, but warming temperature is divided into two steps and carries out, effectively can control the severe degree of reacting on the one hand, ensure the security of reaction, twice intensification is carried out being incubated the integrity that ensure that reaction after terminating again on the other hand.
(4) when reduction reaction of the present invention terminates rear recycling design, press filtration after first reacted material being cooled to 40 DEG C ~ 45 DEG C, then reclaim catalyzer with solvent wash, merging filtrate and washings carry out precipitation operation recycling design, and solvent is reusable after rectifying tower process is reclaimed again.
(5) industrialized process for preparing of 1,8-diaminonaphthalene of the present invention is by the material hot wash after precipitation, then by after liquid-liquid separation, organic phase enters rectifying tower separating-purifying, obtains highly purified 1,8-diaminonaphthalene at tower top, the purity of 1,8-diaminonaphthalene is higher than 99.5%; At the bottom of tower, also obtain purity in addition higher than the 1,5-diaminonaphthalene of 91%, create additional economic worth.
Embodiment
(embodiment 1)
The industrialized process for preparing of 1, the 8-diaminonaphthalene of the present embodiment comprises the following steps:
1. to agitator, thermo detector, reflux exchanger, high-order dropping in the 5000L enamel reaction still of storage tank adds prefabricated catalyzer 70kg, tide product dinitronaphthalene (wherein the quality of dinitronaphthalene is 700kg) and etoh solvent 2500L, then turn on agitator, after under whipped state, in still, material is warming up to 65 DEG C ~ 75 DEG C (in the present embodiment being 70 DEG C), slowly drip the hydrazine hydrate 520kg of 80.1% ~ 100% (being 100% in the present embodiment) at such a temperature, time for adding 5 hours, hydrazine hydrate dropwises and continues to be warming up to 75 DEG C ~ 90 DEG C (in the present embodiment being 75 DEG C) to material in reactor, insulation reaction 3 ~ 8 hours (being 5 hours in the present embodiment) stopped reaction afterwards at such a temperature.
The damp product dinitronaphthalene added through high performance liquid chromatography, detect hereinafter referred to as HPLC, records 95%, 1, the 5-dinitronaphthalene that 1,8-dinitronaphthalene accounts for nitro-naphthalene total mass and accounts for 4.7% of nitro-naphthalene total mass.
Organic solvent used when described dinitronaphthalene tide product refer to and refine containing mixed dinitronaphthalene in dinitronaphthalene raw material, namely naphthalene nitrated after the dinitronaphthalene mixture that obtains refine after drying operation is not carried out to the refining product obtained; After refining, in dinitronaphthalene tide product, solvent accounts for 5% ~ 15% of damp product total mass.The solvent comprised in dinitronaphthalene tide product can be methyl alcohol, ethanol, DMF or toluene.
In the dinitronaphthalene product obtained after usual naphthalene nitration reaction terminates, the content of 1,8-dinitronaphthalene is the content of about 55%, 1,5-dinitronaphthalene is about 31%, and other nitro compounds account for about 4%, water 10%.Therefore the dinitronaphthalene tide product that the present embodiment uses be by nitrated for naphthalene obtain containing 1,5-dinitronaphthalene, 1, the aqueous mixture of 8-dinitronaphthalene and other nitro-compound directly carries out refining removal major part 1, after 5-dinitronaphthalene, the purity requirement detecting 1,8-dinitronaphthalene is the >=95% damp product dinitronaphthalene raw material used as the preparation method of the present embodiment; The purity of 1,8-dinitronaphthalene refers to the content of 1,8-dinitronaphthalene in nitro compounds herein, does not consider water and organic solvent.
The method for prefabricating of wherein prefabricated catalyzer is dissolved in water by ferric chloride hexahydrate, is dispersed in by gac in alkaline aqueous solution and obtains the suspension liquid sodium hydroxide solution of 8 ~ 12 (alkaline aqueous solution in the present embodiment to be pH value be); Then poured into by ferric chloride Solution in gac suspension liquid, the mass ratio of iron(ic) chloride and gac is 1: 2 ~ 5; After stirring, mixture filters, and filters after the filter cake obtained is dried and is catalyzer, stand-by.During reaction, the mol ratio of dinitronaphthalene and hydrazine hydrate is 1: 3 ~ 4, and the consumption of catalyzer is 2% ~ 10% of dinitronaphthalene quality in dinitronaphthalene wet feed.
Solvent, except ethanol, can also be methyl alcohol, DMF, or the mixed solvent that methyl alcohol, ethanol, DMF form with toluene respectively.
2. by step 1. reacted material be cooled to 40 DEG C of then press filtrations, wash the catalyzer that press filtration obtains with a small amount of ethanol, washings and filtered liquid merge as feed liquid process.
3. the feed liquid 2. obtained step is sent into still kettle and is carried out decompression precipitation recycling design, and the solvent that decompression precipitation obtains is sent in rectifying tower after process, and recycling design is reusable.
Above-mentioned decompression precipitation parameter is: pressure-0.050 ~-0.070Mpa, still temperature 50 DEG C ~ 80 DEG C.
During the solvent distillation that above-mentioned decompression precipitation obtains, the stage number of rectifying tower is 60, and feed liquid feeding temperature is 30 DEG C, and feed plate is the 30th piece; Trim the top of column ratio is 1: 6, and overhead condenser pressure is 0.098MPa; The ethanol that tower top is recycled.
4. in the feed liquid after step 3. precipitation, add 50 DEG C ~ 80 DEG C (in the present embodiment being 75 DEG C) hot water carry out washing layering, upper strata is aqueous phase, and lower floor is feed liquid phase, and the volume of hot water is 1 ~ 5 times (being 3 times) of the material liquid volume after precipitation in the present embodiment.
The feed liquid obtained by separatory sends into rectifying in rectifying tower mutually, rectifying obtains: tower top 1,8-diaminonaphthalene finished product 460kg(1,8-diaminonaphthalene is 99.6% through HPLC detection level), byproduct 1,5-diaminonaphthalene 21kg(1 at the bottom of tower, it is 91% that 5-diaminonaphthalene enters HPLC detection level), the yield of 1,8-diaminonaphthalene is 96.46%; The total recovery of 1,8-diaminonaphthalene and 1,5-diaminonaphthalene is 95.4%.
During rectifying, the stage number of rectifying tower used is 60, and feed liquid feeding temperature is 80 DEG C, and feed plate is the 30th piece; Trim the top of column ratio is 1: 6, and overhead condenser pressure is 0.098MPa.
Because the present embodiment is to used 1, the requirement of 8-dinitronaphthalene raw material is 1, the purity requirement of 8-dinitronaphthalene is >=95%, and solvent used when can refine with water and mixed dinitronaphthalene in raw material, therefore by nitrated for naphthalene obtain containing 1,5-dinitronaphthalene, 1, the damp product mixture of 8-dinitronaphthalene and other nitro-compound directly carries out refining removal major part 1, after 5-dinitronaphthalene, detect the purity requirement of 1,8-dinitronaphthalene in nitro compounds and be >=95% just can be used as the dinitronaphthalene raw material that preparation method of the present invention uses.Because naphthalene is nitrated, refining after product without the need to drying, the preparation process of 1,8-dinitronaphthalene decreases dry link, saves the energy, avoids the danger that the long-term localized hyperthermia of nitro compounds causes simultaneously.
The treating process of naphthalene nitration reaction and mixed dinitronaphthalene is as follows:
Carry out nitration reaction with nitration mixture after naphthalene being dissolved in organic solvent and obtain mixed dinitronaphthalene, the known method that the nitration reaction of naphthalene can refer to this area carries out.Described organic solvent is chloroform, ethylene dichloride or tetracol phenixin.Containing 1,8-dinitronaphthalene 60%, 1,5-dinitronaphthalene 35%, other nitro compounds 5% in the nitro compounds that the mixed dinitronaphthalene tide product that the present embodiment obtains detect wherein through high performance liquid chromatography.The moisture mixed dinitronaphthalene obtained, without the need to drying, treats refinement treatment.
Obtained mixed dinitronaphthalene is carried out refining to remove most 1,5-dinitronaphthalene and other nitro compounds.
Add to agitator, reflux exchanger, thermo detector, high-order dropping in the reactor of storage tank the mixed dinitronaphthalene tide product and mixed solvent that nitration reaction obtains successively time refining, the weight ratio of mixed dinitronaphthalene and mixed solvent is 1: 1.5 ~ 5.Described mixed solvent be toluene with in DMF (DMF), methyl alcohol, ethanol one or both, two or more mix after the solvent that obtains.Mixed solvent in the present embodiment is mixed to get by toluene and ethanol equal-volume.
Turn on agitator, is warming up to 80 DEG C ~ 120 DEG C and makes nitro compounds dissolve rear insulation 1 ~ 2 hour completely by material in still.By material slow cooling to 30 DEG C in still after insulation terminates, have crystal to separate out, this crystal is 1,5-dinitronaphthalene; First time suction filtration is carried out to the material after cooling, in the first time filtrate that obtains of suction filtration, major part is 1,8-dinitronaphthalene, dinitronaphthalene tide product are obtained by solvent recrystallization by after filtrate precipitation, dinitronaphthalene tide product detect through high performance liquid chromatography, and record that 1,8-dinitronaphthalene accounts for nitro-naphthalene total mass 95%, 1,5-dinitronaphthalene accounts for 4.7% of dinitronaphthalene total mass.
(embodiment 2)
All the other are identical with embodiment 1 for the industrialized process for preparing of 1, the 8-diaminonaphthalene of the present embodiment, and difference is:
Step 1. in the solvent that adds in reactor be methyl alcohol, dosage is 2500L.
Step 2. in methyl alcohol, the catalyzer that press filtration obtains is washed.
Step 3. recovered solvent is methyl alcohol.
Step 4. rectifying obtains: tower top 1,8-diaminonaphthalene finished product 463kg(1, and it is 99.5% that 8-diaminonaphthalene enters HPLC detection level), byproduct 1,5-diaminonaphthalene 20kg(1 at the bottom of tower, it is 92.3% that 5-diaminonaphthalene enters HPLC detection level).
(embodiment 3)
All the other are identical with embodiment 1 for the industrialized process for preparing of 1, the 8-diaminonaphthalene of the present embodiment, and difference is:
1. under room temperature, dry product dinitronaphthalene 700Kg(1 is added successively to agitator, thermo detector, reflux exchanger, high-order dropping in the 5000L enamel reaction still of storage tank
,8 dinitronaphthalene are 98.5% through HPLC detection level), prefabricated catalyzer 70kg and the mixed solvent that is made up of 2000L ethanol and 500L toluene, open stirring and make material in still be warming up to 70 DEG C.In reactor, drip the hydrazine hydrate 610kg of 85% at such a temperature, time for adding is 4 hours.After hydrazine hydrate dropwises, material in still is continued to be warming up to 79 DEG C, stopped reaction after being then incubated 4 hours.
2. by step 1. reacted material be cooled to 45 DEG C, press filtration reclaim catalyzer, wash the catalyzer that press filtration obtains with a small amount of ethanol, the filtrate merging of washings and press filtration gained sends into distillating recovering solvent in still kettle.
3. after distillation, slough in the material after solvent the hot water adding 70 DEG C and carry out washing layering, after stirring, insulation leaves standstill 0.5 hour, now upper strata is aqueous phase, and lower floor is feed liquid phase, and the feed liquid obtained after separatory sends into rectifying in rectifying tower mutually, rectifying obtains: tower top 1,8-diaminonaphthalene finished product 470.5kg, it is 99.5% that 1,8-diaminonaphthalene enters HPLC detection level, the yield of 1,8-diaminonaphthalene is 94.1%.
During rectifying, the stage number of rectifying tower used is 100, and feed liquid feeding temperature is 90 DEG C, and feed plate is the 50th piece; Trim the top of column ratio is 1: 8, and overhead condenser pressure is 0.098MPa.
Reduction reaction of the present invention terminates first to carry out precipitation operation afterwards, and then in the feed liquid after precipitation, add hot water and carry out washing layering, upper strata is aqueous phase, and lower floor is feed liquid phase, the rectifying of feed liquid phase is obtained 1, the 8-diaminonaphthalene of content more than 99.5%.
(embodiment 4)
All the other are identical with embodiment 3 for the industrialized process for preparing of 1, the 8-diaminonaphthalene of the present embodiment, and difference is:
Step 1. in the solvent that adds in reactor be the DMF of 2500L.
Step 2. in DMF, the catalyzer that press filtration obtains is washed.
Step 3. recovered solvent is DMF.
Step 4. rectifying obtains: tower top 1,8-diaminonaphthalene finished product 472.0kg, 1,8-diaminonaphthalene is 99.45% through HPLC detection level.Product yield is 94.4%.
Claims (4)
1. an industrialized process for preparing for 8-diaminonaphthalene, is characterized in that comprising the following steps:
1. catalyzer, dinitronaphthalene and solvent is added successively to agitator, thermo detector, reflux exchanger, high-order dropping in the enamel reaction still of storage tank, then turn on agitator, material in still is made to be warming up to 65 DEG C ~ 70 DEG C under whipped state, the hydrazine hydrate of 80.1% ~ 100% is slowly dripped at such a temperature in 3 ~ 8 hours, hydrazine hydrate dropwises and continues to be warming up to 75 DEG C ~ 90 DEG C to material in reactor, be incubated 3 ~ 8 hours, terminate reaction; The mol ratio of dinitronaphthalene and hydrazine hydrate is 1: 3 ~ 4, and the quality of catalyzer is 2% ~ 10% of dinitronaphthalene quality, and the quality of solvent is 2 ~ 5 times of dinitronaphthalene quality; In the dinitronaphthalene wherein added in reactor, the purity of 1,8-dinitronaphthalene is more than or equal to 95%;
Described catalyzer is first dissolved in water by ferric chloride hexahydrate, is dispersed in alkaline aqueous solution by gac and obtains suspension liquid; Then poured into by ferric chloride Solution in gac suspension liquid, the mass ratio of iron(ic) chloride and gac is 1: 2 ~ 5; After stirring, mixture filters, stand-by as catalyzer after filtering the filter cake oven dry obtained;
Described solvent is methyl alcohol, ethanol or DMF, or the mixed solvent that methyl alcohol, ethanol, DMF form with toluene respectively;
2. press filtration after 1. reacted material is cooled to 40 DEG C ~ 45 DEG C by step, carry out washing and recycling to the catalyzer that press filtration obtains, washings and filtered liquid merge as feed liquid process;
3. the feed liquid 2. obtained step carries out decompression precipitation recycling design;
4. in the feed liquid after step 3. precipitation, add 50 DEG C ~ 80 DEG C hot water carry out washing layering, upper strata is aqueous phase, and lower floor is feed liquid phase, and the feed liquid obtained by separatory sends into rectifying in rectifying tower mutually, and tower top obtains 1,8-diaminonaphthalene of purity >=99.5%.
2. the industrialized process for preparing of 1,8-diaminonaphthalene according to claim 1, is characterized in that: the dinitronaphthalene that 1. step adds in reactor is damp product or dry product; Comprise water and organic solvent in described dinitronaphthalene tide product, organic solvent is methyl alcohol, ethanol, DMF or toluene.
3. the industrialized process for preparing of 1,8-diaminonaphthalene according to claim 1, is characterized in that: step is 2. after press filtration, and carry out washing and recycling with a small amount of methyl alcohol, ethanol or DMF to the catalyzer that press filtration obtains, washings and filtered liquid merge as feed liquid process.
4. the industrialized process for preparing of 1,8-diaminonaphthalene according to claim 3, is characterized in that: the step 3. solvent that obtains of feed liquid decompression precipitation is sent in rectifying tower and processed, recycling design as step 1. in solvent use; During the solvent distillation that decompression precipitation obtains, the stage number of rectifying tower is 40 ~ 80, and feed liquid feeding temperature is 28 DEG C ~ 35 DEG C, and feed plate is 20th ~ 40 pieces; Trim the top of column ratio is 1: 4 ~ 10, and overhead condenser pressure is 0.098MPa ~ 1MPa; The solvent that tower top is recycled.
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| CN101823968B (en) * | 2010-05-21 | 2013-01-09 | 南通龙翔化工有限公司 | Method for preparing 1,8-diaminonaphthalene by reducing 1,8-dinitronaphthalene with hydrazine hydrate |
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