CN107162919A - Energy-efficient, environmentally friendly novel diamino diphenyl ether production line - Google Patents
Energy-efficient, environmentally friendly novel diamino diphenyl ether production line Download PDFInfo
- Publication number
- CN107162919A CN107162919A CN201710569660.5A CN201710569660A CN107162919A CN 107162919 A CN107162919 A CN 107162919A CN 201710569660 A CN201710569660 A CN 201710569660A CN 107162919 A CN107162919 A CN 107162919A
- Authority
- CN
- China
- Prior art keywords
- reaction
- energy
- diphenyl ether
- production line
- efficient
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of energy-efficient, environmentally friendly novel diamino diphenyl ether production line, including input main material, flow, production three parts of thing and condensation reaction, reduction reaction, exquisite purification and crushing packing four processes.It is characterized in that by from low toxicity, efficiently, solvent, the catalyst reused, the closing flow of no air and impurity intervention, produce >=99.9% the diaminodiphenyl ethers of 4,4 ＇ mono-.The present invention compared with prior art, with production cable architecture and constitutes simple, and reaction link is few, and the used time is short, the features such as efficiency high, also repeat that reactivity is high, blowdown is few, toxicity is low with solvent, catalyst, energy-saving and environmental protection, the important advantage such as safe and cost-effective.
Description
First, technical field
The present invention relates to industrial chemicals production, and in particular to a kind of energy-efficient, environmentally friendly novel diamino diphenyl ether life
Producing line.
2nd, background technology
Diaminodiphenyl ether is as raw material, additive, intermediate and crosslinking agent, for production specific function and property
The industries such as electromechanics, electronics, plastics, resin, dyestuff, spices and product, and research and development more powerful and special nature and function are new
Product, all has and occupies special and critical role that is can not be substituted and effect.It can realize and reach above-mentioned purpose, key exists
In high cleanliness fine work can be produced.Prior art production diaminodiphenyl ether generalized flowsheet be：1st, condensation reaction will be right
Condensation reaction is added according to this under p-nitrophenol sodium, para-nitrochloro-benzene, dimethyl acetamide, sodium hydrogensulfite, potassium chloride stirring
Kettle simultaneously heats up, maintain the lower reaction of 210-215 DEG C of stirring 24 hours again through vacuum distillation, steam distillation, 4,4 ＇ of suction strainer washing acquisition-
Dinitro diphenyl ether.2nd, butanol, ammonium chloride, iron filings are added reduction reaction kettle by reduction reaction, and stirring heating is lower to add 4,4 ＇-two
Itrodiphenyl ethers, adds second batch, and the 3rd batch of iron filings catalysis maintains 100 DEG C to react 1.5 hours, adds sodium hydrogensulfite, stir
Mix decrease temperature crystalline after dissolving, filtering, the obtained 4,4 ＇-diaminodiphenyl ether product of washing.3rd, purification is refined：Water and hydrochloric acid are added
Dissolving tank, the lower addition 4 of stirring, 4 ＇-diaminodiphenyl ether crude product and citric acid, sodium hydrogensulfite, activated carbon, heating stirring are mixed
Filtering is transferred to neutralization chamber afterwards, adds sodium hydrogensulfite and ammoniacal liquor, and regulation pH value to 8-9, cooling is maintained to the diaminourea two of 4,4 ＇ mono-
Phenylate crystallization is separated out, filtering, is dried in vacuo after obtaining filter cake, washing suction filtration.The dry diaminodiphenyl ethers of 4,4 ＇ mono- are added
Sublimator, heating distillation, is transferred to crystallisation chamber crystallisation by cooling, gets product.The problem of above-mentioned production process is present be：1st, ring is produced
Section is more, node is maintained and interval time length, efficiency are low；2nd, condensation reaction, reduction reaction and refined purification process are numerous and diverse, and regulation and control are difficult
Degree is big, technical requirements are high.3rd, its process heating, cooling, constant temperature time are long, and the number of occurrence is more, energy consume is big.4th, produced in the middle of it
Product and crude product washing times are more, water consumption is big, product sewage is more, follow-up water process burden weight；Generation oxidation iron cement solid waste, seriously
Pollute environment.5th, open reactive and process node are more, and escaping gas, which overflows, loses serious, pollution atmospheric environment.6th, distil
Process technology condition requires high, and risk is big, safety factor is more.
3rd, the content of the invention
The purpose of the present invention is that there is provided a kind of energy-efficient, environmentally friendly new diamino with deficiency for above technical problem
Yl diphenyl ether production line.
The purpose of the present invention is achieved through the following technical solutions：
A kind of energy-efficient, environmentally friendly novel diamino diphenyl ether production line, including by production line it is longitudinally divided put into
Main material, flowchart process, three parts of product and laterally to produce 4,4 ＇ of thing-dinitro diphenyl ether, 4,4 ＇-diaminourea two
Condensation reaction, reduction reaction, refined purification and drying that phenylate crude product, >=99.9%4,4 ＇-diaminodiphenyl ether, finished product are divided
Crushing packing four-stage, it is characterized in that strict measurement input para-nitrochloro-benzene, Sodium p-nitrophenoxide, dimethyl second in proportion
Acid amides is prepared after composite solution, first through shunting the crystallization water that distillation system removing free water and Sodium p-nitrophenoxide contain,
Catalyst potassium chloride is added under anhydrous condition and carries out condensation reaction, 4,4 ＇-dinitro diphenyl ether are made in crystallization filtration；With dimethyl
Acetamide dissolves again, adds activated carbon of sorbent filtration and eliminates after impurity, injection reducing agent hydrogen and noble metal catalyst enter
4,4 ＇-diaminodiphenyl ether crude product are produced in row reduction reaction, filtering distillation；4,4 ＇ produced-diaminodiphenyl ether dissolving crude product
Into methanol and toluene Mixed Solvent, through filtering, distillation, crystallization and purification, suction filtration separation solvent obtains >=99.9%4,4 ＇-diamino
Yl diphenyl ether；Re-dry packaging turns into finished product.
It is characterized in that from the condensation reaction after raw material input, the suction filtration of reduction reaction process and refined purification process,
Separate before solvent, be, in closing, nitrogen to be filled with after vacuumizing, remove air and moisture content and the negative pressure or normal with air exclusion
Carried out under pressure condition, its pressure value is that vavuum pump adjusts, rushes nitrogen, equipment sealing realization.
It is characterized in that dissolving after material input, reaction, crystallization, the gradient of temperature in still-process and control room are by anti-
Infusion and cyclic high-temperature steam, deep fat, cold oil valency matter or cooling water in the heating and cooling interlayer of kettle, distillation still, filtering tank are answered, is passed through
What the kettle inwall transmission of closing isolation was completed indirectly.
It is characterized in that condensation reaction is to remove the trip that the Sodium p-nitrophenoxide crystallization water and raw material adhesion are carried in separation
From water, carried out under complete anhydrous condition, reduction reaction and refined purification process are to synthesize new unboiled water in continuous elimination reaction
Under conditions of carry out.
It is characterized in that the reducing agent in reduction reaction is the hydrogen of input, catalyst is noble metal catalyst.
The present invention energy-efficient, environmentally friendly novel diamino diphenyl ether production line compared with prior art, with following
Distinguishing feature and advantage：
1st, raw material, solvent, catalyst, adsorbent needed for during condensation reaction, reduction reaction are generally strict meter mark,
Disposable or continuity input after metering, greatly reduces adjustment consumption and exploratory repeatedly input, the ring of adding speed after monitoring
Section less, accurate easily-controllable, time saving and energy saving efficiency high.
2nd, the course of reaction of whole operation is carried out in closing nitrogen environment, and free from admixture is mixed into, odorlessness overflows, reacted without dry
Disturb.
3rd, the species such as input solvent, assisted reaction agent, catalyst, PH nertralizers, adsorbent is few, constitutes simply, association is anti-
It should be generated as few, it is few to produce residue, residual salt impurity and sewage quantity, remove and post processing is simple, pollution level is low.
4th, hydrogen reducing is injected in reduction reaction, reaction is rapider thorough.
5th, condensation reaction is carried out in sewage, reduction reaction in the environment for removing water, and reaction is disturbed less, degree of safety is high.
6th, it is good with precious metal catalyst, effect in reduction reaction, it is also easy to all reclaim repetition use.
7th, the flow scheme that purification process gives up distillation is refined, energy-saving safe risk is low.
8th, washing times are few, water consumption is few, generation sewage is few, water-saving and environmental protection.
9th, above-mentioned factors reason, makes in course of reaction that heating and cooling number of times is few, amplitude is small, the reaction used time is short, energy-conservation is high
Effect.
10th, final products degree of purity can >=99.9%, quality is good.
4th, illustrate
Fig. 1 is the typical process flow schematic diagram of energy-efficient, environmentally friendly novel diamino diphenyl ether production line.
In figure：1 input main material, 2 flows, 3 products, 4 4,4 ＇-dinitro diphenyl ether, 5 4,4 ＇-diaminourea two
The ＇ ' of phenylate crude product, 6 purity >=99.9%4,4-diaminodiphenyl ether, 7 finished products.
5th, embodiment
The present invention is illustrated in further detail below with reference to Figure of description：
Energy-efficient, the environmentally friendly novel diamino diphenyl ether production line of the present invention is in the gloomy insulation system of Dongying city hat
Product Co., Ltd《10000T/ recrystallization methods produce high-purity diaminodiphenyl ether projects》During research and development and implement.
As shown in Figure 1：Energy-efficient, environmentally friendly novel diamino diphenyl ether production line is to generate 4,4 ＇-dinitro of generation
Yl diphenyl ether 4, the diaminodiphenyl ether crude products 5 of 4,4 ＇ mono-, purity >=99.9%4,4 ＇-diaminodiphenyl ether 6 and product 7 are divided into
Condensation reaction, reduction reaction, refined purification and dry packing four-stage, it is general to put into main material 1, flow 2 and product 3
Include as three parts.
Line design is generated, installs, debugging, during input, link put into again in input main material 1 and product 3,
Accurate measuring device is provided with, to the link stage of condensation reaction, reduction reaction and refined purification, closed operation is both designed as
Circulation process, and install combine the vacuum pumping pump being used alone and nitrogen input substitute air device, to need temperature adjustment, insulation
Reactor, dissolution kettle, distillation still, filtering tank, using be provided with for high-temperature steam, the deep fat such as cooling water, cold oil circulation control
Warm interlayer.The fractional distillation dewatering system for being completely separated and removing free moisture content and the crystallization water is set up to condensation reaction kettle, pair also
Reduction reaction kettle and distillation still in former course of reaction are provided with continuously detaching vavuum pump and the pressurization of the new unboiled water of reaction synthesis
Nitrogen charging air pump.
In production process：From dimethyl acetamide be solvent, toxicity is low, highly polar, solubility is big, reaction speed is fast,
Efficiency high, degree of safety are high.Temperature is low, pressure is low, degree of safety needed for hydrogenating reduction, noble metal catalyst, reaction in reduction reaction
It is high.Refined purification obtains >=99.9%4,4 ＇-diaminodiphenyl ether finished product using mixed solvent dissolving-recrystallization, substitutes suction filtration and does
Distillation recrystallization technique after dry, efficiency high, energy consumption are low.Condensation reaction, reduction reaction, refine purification process using closing, nitrogen
Air flow is substituted, has evaded reaction generation impurity, artificial and environment often enters magazine, provided reliably for high-purity product
Guarantee.
It is the known technology of this industry technical staff in addition to the technical characteristic described in specification.
Claims (5)
1. a kind of energy-efficient, environmentally friendly novel diamino diphenyl ether production line, including by production line it is longitudinally divided put into master
Material, flowchart process, three parts of product and transverse direction is wanted to produce 4,4 ＇ of thing-dinitro diphenyl ether, 4,4 ＇-diaminourea hexichol
Condensation reaction, reduction reaction, refined purification and dry bag that ether crude product, >=99.9%4,4 ＇-diaminodiphenyl ether, finished product are divided
Four-stage is filled, it is characterized in that strict measurement input para-nitrochloro-benzene, Sodium p-nitrophenoxide, dimethyl acetamide system in proportion
After standby mixed solution, first through shunting the crystallization water that distillation system removing free water and Sodium p-nitrophenoxide contain, without water bar
Catalyst potassium chloride is added under part and carries out condensation reaction, 4,4 ＇-dinitro diphenyl ether are made in crystallization filtration；With dimethyl acetamide
Dissolve again, add activated carbon of sorbent filtration and eliminate after impurity, injection reducing agent hydrogen and noble metal catalyst are reduced
4,4 ＇-diaminodiphenyl ether crude product are produced in reaction, filtering distillation；4,4 ＇ produced-diaminodiphenyl ether and methanol and toluene are mixed
After bonding solvent dissolving, evaporated by filtration, crystallisation by cooling is purified, suction filtration separation solvent obtains >=99.9%4,4 ＇-diaminourea hexichol
Ether；Re-dry packaging turns into finished product.
2. energy-efficient, the environmentally friendly novel diamino diphenyl ether production line according to claim 1, it is characterized in that from original
It is in closing before condensation reaction after material input, the suction filtration of reduction reaction process and refined purification process, separation solvent
, it is filled with nitrogen after vacuumizing, removes air and moisture content and with being carried out under the negative pressure or atmospheric pressure state of air exclusion, its pressure
Value is that the nitrogen-sealed of vavuum pump regulation is realized.
3. energy-efficient, the environmentally friendly novel diamino diphenyl ether production line according to claim 1, it is characterized in that material
Dissolve, react after input, crystallization, the gradient of temperature in still-process and control room be by reactor, distillation still, filtering tank
Infusion and cyclic high-temperature steam, deep fat, cold oil valency matter or cooling water in heating and cooling interlayer, are transmitted by the kettle inwall for closing isolation
Complete indirectly.
4. energy-efficient, the environmentally friendly novel diamino diphenyl ether production line according to claim 1, it is characterized in that condensation
Reaction is to remove the free water that the Sodium p-nitrophenoxide crystallization water and raw material adhesion are carried in separation, under complete anhydrous condition
Carry out, reduction reaction and refined purification process are carried out under conditions of continuous elimination reaction synthesizes new unboiled water.
5. energy-efficient, the environmentally friendly novel diamino diphenyl ether production line according to claim 1, it is characterized in that reduction
Reducing agent in reaction is the hydrogen of input, and catalyst is noble metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710569660.5A CN107162919B (en) | 2017-07-13 | 2017-07-13 | A kind of production method of diaminodiphenyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710569660.5A CN107162919B (en) | 2017-07-13 | 2017-07-13 | A kind of production method of diaminodiphenyl ether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107162919A true CN107162919A (en) | 2017-09-15 |
| CN107162919B CN107162919B (en) | 2019-03-19 |
Family
ID=59823954
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710569660.5A Active CN107162919B (en) | 2017-07-13 | 2017-07-13 | A kind of production method of diaminodiphenyl ether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107162919B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108752222A (en) * | 2018-08-20 | 2018-11-06 | 万达集团股份有限公司 | A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers |
| CN110028414A (en) * | 2019-04-26 | 2019-07-19 | 山东欧亚化工有限公司 | A method of extracting 4,4 '-diaminodiphenyl ethers of separation from concentration kettle defective material |
| CN114591178A (en) * | 2022-03-17 | 2022-06-07 | 宁夏德昊科技产业有限公司 | ODA production process and production system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1334659A (en) * | 1971-07-26 | 1973-10-24 | Hall Co Howard | Preparation of substituted diphenyl ethers |
| CN102391136A (en) * | 2011-10-27 | 2012-03-28 | 东营市冠森绝缘制品有限公司 | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process |
| CN102850229A (en) * | 2012-07-24 | 2013-01-02 | 万达集团股份有限公司 | Process for preparing 4,4'-diaminodiphenyl ether by hydrogenation reduction method |
-
2017
- 2017-07-13 CN CN201710569660.5A patent/CN107162919B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1334659A (en) * | 1971-07-26 | 1973-10-24 | Hall Co Howard | Preparation of substituted diphenyl ethers |
| CN102391136A (en) * | 2011-10-27 | 2012-03-28 | 东营市冠森绝缘制品有限公司 | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process |
| CN102850229A (en) * | 2012-07-24 | 2013-01-02 | 万达集团股份有限公司 | Process for preparing 4,4'-diaminodiphenyl ether by hydrogenation reduction method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108752222A (en) * | 2018-08-20 | 2018-11-06 | 万达集团股份有限公司 | A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers |
| CN110028414A (en) * | 2019-04-26 | 2019-07-19 | 山东欧亚化工有限公司 | A method of extracting 4,4 '-diaminodiphenyl ethers of separation from concentration kettle defective material |
| CN110028414B (en) * | 2019-04-26 | 2022-04-19 | 山东欧亚化工有限公司 | Method for extracting and separating 4,4' -diaminodiphenyl ether from concentrating kettle residue |
| CN114591178A (en) * | 2022-03-17 | 2022-06-07 | 宁夏德昊科技产业有限公司 | ODA production process and production system |
| CN114591178B (en) * | 2022-03-17 | 2023-08-29 | 宁夏德昊科技产业有限公司 | ODA production process and production system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107162919B (en) | 2019-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5850550B2 (en) | Method for producing taurine | |
| CN101139338B (en) | Preparation of 2,2'-disulfo-dibenzopyrene by oxygen process based on 2-mercaptan benzothiazole ammonia salt | |
| CN107162919A (en) | Energy-efficient, environmentally friendly novel diamino diphenyl ether production line | |
| TW200714639A (en) | Process and equipment for the decomposition and recovery of isocyanate compounds | |
| CN103626240B (en) | Lower concentration complexity prepares the method for ruthenium trichloride containing ruthenium waste liquid | |
| CN111330412B (en) | System and process for absorbing and purifying byproduct hydrogen chloride gas in chlorination section into acid | |
| CN104817588A (en) | Preparation method of ethyl chloride | |
| CN104032128A (en) | Method for producing electrolytic nickel by leaching and purifying manganese-containing nickel hydroxide | |
| CN105084359B (en) | A kind of method that formic acid dehydration industry prepares high-purity CO | |
| CN101891164A (en) | Method for purifying cubic boron nitride | |
| CN105218705A (en) | A kind of double enzymolysis legal system that utilizes is for the method for heparin sodium | |
| CN104003910A (en) | Method for extracting m-phthalic acid-5-sodium sulfonate from ternary-monomer industrial waste water | |
| CN217627632U (en) | Preparation system for directly producing electronic-grade nitric acid from ammonia gas | |
| CN105273760A (en) | Waste water zero-discharge acetylene production technology | |
| CN213231531U (en) | Continuous nitric oxide production device | |
| CN109180605A (en) | The method of the direct synthetic rubber vulcanization accelerator TBBS of resin in waste water | |
| WO2014183381A1 (en) | Method for caustic purification of silicon carbide filter cake | |
| CN107973711A (en) | A kind of method of Simulation moving bed separating glucose acid mother liquid of sodium | |
| CN108484423A (en) | A method of isolating and purifying l-Alanine from l-Alanine zymotic fluid | |
| CN104610407B (en) | The process for purification of hydrocortisone acetate | |
| CN108727297A (en) | A kind of hydrogen peroxide oxidation one-step synthesis technique of rubber accelerator dibenzothiazyl disulfide | |
| CN103496722B (en) | Method for preparing high-purity sodium sulfite through supercritical hydrothermal reduction | |
| CN207478574U (en) | A kind of process units of thiocarbohydrazide | |
| CN103435070B (en) | A kind of from containing the method reclaiming product the waste residue of Sodium Fluoride | |
| CN102345014B (en) | Method for preparing elementary copper, copper hydroxide and sodium chloride through dye waste residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |