CN206127174U - 3, 4 diaminotoluene's synthesizer - Google Patents

Abstract

The utility model relates to a 3, 4 diaminotoluene's synthesizer, characterized by: including the methyl alcohol storage tank, dissolving kettle, the high -pressure hydrogenation cauldron, piptonychia mellow wine cauldron, rectifying still and finished product receiving slit, the methyl alcohol storage tank passes through methanol pump and connects the methyl alcohol elevated tank, dissolving kettle is connected to the discharge end of methyl alcohol elevated tank, dissolving kettle's discharge end changes the feed end that the high -pressure hydrogenation cauldron is connected to the material pump through dissolving liquid, the input of filter press is connected to the discharge end of high -pressure hydrogenation cauldron, the feed end of piptonychia mellow wine cauldron is connected to the output of filter press, the feed end of rectifying still is connected to the discharge end of piptonychia mellow wine cauldron, the feed end of rectifying column is connected to the discharge end of rectifying still, the feed end of rectification top of the tower condenser is connected to the discharge end of rectifying column, the dehydration receiving slit is connected to the dehydration discharge end of rectification top of the tower condenser, the finished product receiving slit is connected to the finished product discharge end of rectification top of the tower condenser. Adopt this synthesizer to synthesize, technology is advanced reasonable, low in production cost, and synthesis route is short, and product purity is high.

Description

The synthesizer of 3,4- diaminotoluenes

Technical field

This utility model is related to the synthesizer of one kind 3,4- diaminotoluenes, belongs to chemical industry organic synthesiss equipment and technology neck Domain.

Background technology

3,4- diaminotoluenes（Also known as 4- methyl-o-phenylenediamines）It is a kind of important organic intermediate, for synthesizing top grade Organic pigment scattered fluorescent yellow and synthesis metal（Such as silver, copper, lead, nickel, zinc）Antirust agent and corrosion inhibiter（5- methylbenzene a pair of horses going side by side three Nitrogen azoles）, it is widely used in antirust oil（Fat）In class product, it is used for the vapour phase inhibitor circulating water treatment agent of copper and copper alloy, Motor vehicle antifreeze fluid, macromolecule stabilizer, plant growth regulator, lube oil additive, UV absorbent etc..

In prior art, the synthetic method of 3,4- diaminotoluenes has two kinds, one kind be adopt Red G Salt for Raw material, Jing sodium sulfide reducings, reducing solution separates removing moisture content after sulfur-containing waste water and obtains 3,4- diaminotoluene finished products, and content 92% is left The right side, yield 90% or so, 8 tons or so of synthetic route product waste discharge per ton；Another kind of method is to first using adjacent nitro Aniline is raw material, and Jing iron powder reducings, reducing solution removes after filtering moisture content and obtains 3,4- diaminotoluene finished products, content 92%-95% Left and right, yield 87%-90% or so, 10 tons of synthetic route product waste discharge per ton.Two kinds of synthesis 3,4- diaminourea first of the above The method high cost of benzene, seriously polluted, finished product content is low, and outward appearance sepia, oxidation stain in air, quality is unstable.

The content of the invention

The purpose of this utility model is to overcome the deficiencies in the prior art, there is provided the conjunction of one kind 3,4- diaminotoluenes Into device, synthesized using the synthesizer, technique is advanced, and rationally low production cost, synthetic route is short, and product purity is high.

According to the technical scheme that this utility model is provided, the synthesizer of 3, the 4- diaminotoluenes is characterized in that：Bag Include methanol storage tank, dissolution kettle, high-pressure hydrogenation kettle, separating methanol kettle, rectifying still and finished product receiving slit, methanol storage tank discharging opening connection first The input of alcohol pump, the outfan of methanol pump connects the feed end of methanol head tank, the discharge end connection dissolving of methanol head tank The feed end of kettle, the discharge end of dissolution kettle connects the input of lysate transfering material pump, and the outfan connection of lysate transfering material pump is high The feed end of pressure hydrogenation kettle, the discharge end of high-pressure hydrogenation kettle connects the input of filter press, the outfan connection piptonychia of filter press The feed end of alcohol kettle, the discharge end of separating methanol kettle connects the feed end of rectifying still, and the discharge end of rectifying still connects entering for rectifying column Material end, the discharge end of rectifying column connects the feed end of rectifying tower top condenser, the dehydration discharge end connection of rectifying tower top condenser Dehydration receiving slit, the finished product discharge end connection finished product receiving slit of rectifying tower top condenser.

Further, reflux condenser is connected in the dissolution kettle.

Further, methanol distillation column is connected on the separating methanol kettle, the discharge end connection methanol of methanol distillation column is cold The feed end of condenser, the discharging opening of methanol condenser connects respectively the feedback outlet of methanol storage tank and the feedback outlet of methanol distillation column.

This utility model has the advantages that：3,4- diaminotoluenes synthesizer described in the utility model, with neighbour Nitro-p-toluidine is raw material, and methanol is solvent stirring and dissolving in dissolution kettle, and with lysate transfering material pump high-pressure hydrogenation kettle is sent into 3,4- diaminotoluenes are hydrogenated under the effect of catalyst nickel, the material Jing filter presss being hydrogenated with kettle are pressed into into separating methanol with nitrogen Kettle, normal pressure methanol removal（Recovery）Afterwards, material is sucked in rectifying still with vacuum, under reduced pressure water is removed（Go dehydration Receiving slit）, last rectification under vacuum goes out 3,4- diaminotoluenes finished product to finished product receiving slit（Purity is up to 99.5%）.In sum originally 3,4- diaminotoluenes technique made by synthesizer described in utility model is advanced, and rationally low production cost, synthetic route is short, produces Product purity is high（99.5%）The three wastes are few.

Description of the drawings

Fig. 1 is the schematic diagram of the synthesizer of 3,4- diaminotoluenes described in the utility model.

Specific embodiment

With reference to concrete accompanying drawing, the utility model is described in further detail.

As shown in Figure 1：The synthesizer of 3, the 4- diaminotoluenes includes that methanol storage tank 1, methanol pump 2, methanol are high-order Groove 3, reflux condenser 4, dissolution kettle 5, lysate transfering material pump 6, high-pressure hydrogenation kettle 7, filter press 8, separating methanol kettle 9, Methanol Recovery Tower 10, methanol condenser 11, rectifying still 12, rectifying column 13, rectifying tower top condenser 14, dehydration receiving slit 15, finished product receiving slit 16 etc..

As shown in figure 1, the synthesizer of 3,4- diaminotoluenes described in the utility model, including methanol storage tank 1, dissolution kettle 5th, high-pressure hydrogenation kettle 7, separating methanol kettle 9, rectifying still 12 and finished product receiving slit 16, the discharging opening of methanol storage tank 1 connects the defeated of methanol pump 2 Enter end, the feed end of the outfan connection methanol head tank 3 of methanol pump 2, the discharge end of methanol head tank 3 connects dissolution kettle 5 Feed end, the input of the discharge end connection lysate transfering material pump 6 of dissolution kettle 5, the outfan connection high pressure of lysate transfering material pump 6 The feed end of hydrogenation kettle 7, the discharge end of high-pressure hydrogenation kettle 7 connects the input of filter press 8, and the outfan connection of filter press 8 is de- The feed end of methanol kettle 9, the discharge end of separating methanol kettle 9 connects the feed end of rectifying still 12, the discharge end connection essence of rectifying still 12 Evaporate the feed end of tower 13, the feed end of the discharge end connection rectifying tower top condenser 14 of rectifying column 13, rectifying tower top condenser 14 Dehydration discharge end connection dehydration receiving slit 15, the finished product discharge end connection finished product receiving slit 16 of rectifying tower top condenser 14.

Connect reflux condenser 4 in the dissolution kettle 5.

Connect methanol distillation column 10, the discharge end connection methanol condenser of methanol distillation column 10 on the separating methanol kettle 9 11 feed end, the discharging opening of methanol condenser 11 connects respectively the feedback outlet of methanol storage tank 1 and the feed back of methanol distillation column 10 Mouthful.

The course of work of the present utility model：Methanol methanol pump 2 in methanol groove 1 is squeezed into into the Jing of methanol head tank 3 meterings After be put in dissolution kettle 5, open stirring, be slowly added into the Red G Salt of ormal weight, be heated to 50～55 DEG C and stir to complete CL.Then the Red G Salt methanol solution for having dissolved is squeezed in high-pressure hydrogenation kettle 7 with lysate transfering material pump 6, Material has been beaten, and adds the Raney nickel for measuring, and with nitrogen, hydrogen three times are changed respectively.Replacement completion opens stirring and is passed through hydrogen Gas, is warming up to 60 DEG C, starts hydrogenation, and control hydrogenation pressure to 1.5～2.0MPa, temperature 65-75 DEG C, hydrogenation end maintenance 1 is little When, 1 hour is stood, hydrogen is arranged, discharging is pressed into the material Jing filter presss 8 in high-pressure hydrogenation kettle 7 in separating methanol kettle 9 with nitrogen. Normal pressure sloughs methanol to methanol groove（Recovery）, then first existed in the material suction rectifying still 12 in separating methanol kettle 9 with vacuum Slough under reduced pressure water to be dehydrated receiving slit 15, most after Jing rectifications under vacuum obtain 3,4- diaminotoluenes finished product to finished product receiving slit 16, content 99.5%, yield 96.7%

The synthesizer of 3,4- diaminotoluenes described in the utility model, made by 3,4- diaminotoluene production costs Low, product purity is high, and quality is good, and the three wastes are few.

Claims (3)

1. one kind 3, the synthesizer of 4- diaminotoluenes, is characterized in that：Including methanol storage tank（1）, dissolution kettle（5）, high pressure adds Hydrogen kettle（7）, separating methanol kettle（9）, rectifying still（12）With finished product receiving slit（16）, methanol storage tank（1）Discharging opening connects methanol pump（2） Input, methanol pump（2）Outfan connection methanol head tank（3）Feed end, methanol head tank（3）Discharge end connection Dissolution kettle（5）Feed end, dissolution kettle（5）Discharge end connection lysate transfering material pump（6）Input, lysate transfering material pump （6）Outfan connection high-pressure hydrogenation kettle（7）Feed end, high-pressure hydrogenation kettle（7）Discharge end connection filter press（8）Input End, filter press（8）Outfan connection separating methanol kettle（9）Feed end, separating methanol kettle（9）Discharge end connection rectifying still（12） Feed end, rectifying still（12）Discharge end connection rectifying column（13）Feed end, rectifying column（13）Discharge end connection rectification Overhead condenser（14）Feed end, rectifying tower top condenser（14）Dehydration discharge end connection dehydration receiving slit（15）, rectification Overhead condenser（14）Finished product discharge end connection finished product receiving slit（16）.

2. the synthesizer of 3,4- diaminotoluenes as claimed in claim 1, is characterized in that：In the dissolution kettle（5）Upper company Take back flow condenser（4）.

3. the synthesizer of 3,4- diaminotoluenes as claimed in claim 1, is characterized in that：In the separating methanol kettle（9）On Connection methanol distillation column（10）, methanol distillation column（10）Discharge end connection methanol condenser（11）Feed end, methanol condensed Device（11）Discharging opening connect methanol storage tank respectively（1）Feedback outlet and methanol distillation column（10）Feedback outlet.