CN205925041U - 3, 3' dichloro 4, 4' diamino diphenyl methane device of purifing - Google Patents

3, 3' dichloro 4, 4' diamino diphenyl methane device of purifing Download PDF

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Publication number
CN205925041U
CN205925041U CN201620903622.XU CN201620903622U CN205925041U CN 205925041 U CN205925041 U CN 205925041U CN 201620903622 U CN201620903622 U CN 201620903622U CN 205925041 U CN205925041 U CN 205925041U
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China
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chloro
diaminodiphenyl
purifying plant
vacuum pump
distance distiller
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CN201620903622.XU
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Chinese (zh)
Inventor
杨申
钟文清
陈南超
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Shandong Chong Shunxin Mstar Technology Ltd
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Shandong Chongshun Chemical Co Ltd
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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The utility model discloses a 3, 3' dichloro 4, 4' diamino diphenyl methane device of purifing, including stills and the short distance distiller that communicates in proper order, stills's gas exports communicates in proper order has condenser and hold up tank, the short distance distiller still communicates respectively has product groove and raffinate groove, the hold up tank with the short distance distiller still communicates respectively has vacuum unit system. The utility model discloses a device combination has optimized the production process, makes production process become simpler, high efficiency, safety, yield height, and the product purity of production is high, the quality is good, the application is wide, still eliminated the crystallization process and used the low problem unstable with the quality of a large amount of solvents and cauldron formula way of distillation yield, be particularly suitable for the industrial production and promote.

Description

Chloro- 4,4 ' of 3,3 '-two-diaminodiphenyl-methane purifying plant
Technical field
This utility model belongs to technical field of chemical and in particular to a kind of 3,3 '-two chloro- 4,4 '-diaminourea hexichol Methylmethane purifying plant.
Background technology
3,3 '-two chloro- 4,4 '-diaminodiphenyl-methane (MOCA) industrial goods are generally divided into two kinds of specifications, one purity Be only slightly larger than 85% because its outward appearance be faint yellow to yellow, referred to as yellow MOCA, its two be purity more than 98.5%, Its outward appearance is white, so referred to as white MOCA;It is white MOCA using the MOCA that this utility model device manufactures, its purity is higher, More than 99.0% can be reached.
High-purity MOCA (white MOCA), in addition to can apply to typically yellow MOCA range, can also prepare high property Can, in colourless and light color article, because its purity is high, the physical property of its product is more excellent, and its market price is also than common Huang MOCA is high 2~3 times for type, and with the popularization and application of new material and new technique, white MOCA is increasingly favored by market, its city Field demand is increasing year by year.
High-purity MOCA (white MOCA) took organic low boiling alcohols (methanol, ethanol, isopropanol etc.) crystallization legal system in the past Standby, the method exists using a large amount of alcohols solvent dissolvings, and solvent is inflammable thing, has very big potential safety hazard, and It is also easy to produce crystal grain cladding phenomenon in crystallization process, cause purity not reach requirement;Made still distillation into later although still distillation Qualified products can be prepared, but product yield is low, stability is poor, main cause is that the boiling point of MOCA is higher, still distillation Heat time heating time is long, and distillation efficiency is low, causes MOCA to stop for a long time at high temperature, produces carbonization and decomposing phenomenon.
Content of the invention
Technical problem to be solved in the utility model:In view of the shortcomings of the prior art, one kind is provided can to solve to produce Chloro- 4,4 ' of the 3,3 '-two-diaminodiphenyl-methane purifying plant of the problems such as rate is low, stability is poor.
For solving above-mentioned technical problem, the technical solution of the utility model is:Make in nitrogen air-blowing first with distillating still With under, steam the moisture in MOCA, free o-chloraniline (OCA) and low boiling impurity, then material be warming up to a constant temperature Degree enters in short-distance distiller, carries out molecular distillation, the height boiling such as the trimer in separation MOCA and polymer under a high vacuum Point material, and then prepare the white MOCA of high-purity and high-quality.
3,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant, steams including the distillating still being sequentially communicated and short distance Evaporate device;The gaseous phase outlet of described distillating still has been sequentially communicated condenser and dump tank;Described short-distance distiller has also been respectively communicated with Product groove and residual liquid groove;Described dump tank and described short-distance distiller have also been respectively communicated with vacuum pump set system.
Preferably, described vacuum pump set system is also sequentially communicated sour spray column and activated carbon adsorber.
Preferably, described distillating still is the stainless steel cauldron being provided with chuck and agitating device.Its volume be 200~ 2000L, preferably 500~1000L, material is 304,316 or 316L rustless steel, preferably 316 or 316L.
Preferably, described short-distance distiller is molecular still.
Preferably, described short-distance distiller is provided with external heat plate and intracavity coldplate
Preferably, described vacuum pump set system includes vacuum buffer tank, cold-trap surge tank, water circulation vacuum pump, oil Circulation vacuum pump and three-level Roots vaccum pump.
Preferably, described condenser is stainless steel condenser, and dump tank is rustless steel dump tank, product groove is rustless steel Product groove, residual liquid groove are rustless steel residual liquid groove.Apparatus above material be 304,316 or 316L rustless steel, preferably 316 or 316L.
Preferably, the sour spray column that described sour spray column is prepared for polypropylene, activated carbon adsorber is prepared for polypropylene Activated carbon adsorber;Above stream oriented device or with fiberglass, polypropylene random copolymer material prepare, preferably poly- third Alkene, polypropylene random copolymer material.
Due to employing technique scheme, the beneficial effects of the utility model are:
1. equipment Combinatorial Optimization of the present utility model production process, make production process become simpler, efficiently, safety, High income;
2. the product purity height of production, quality better, application are wide;
3. eliminated that crystallization process uses a large amount of solvents and still distillation method yield is low and the unstable problem of quality, especially suitable Close industrialized production to promote.
Brief description
With reference to the accompanying drawings and examples this utility model is further illustrated.
Fig. 1 is the equipment flowsheet schematic diagram of this utility model embodiment;
Wherein, 1. distillating still;2. condenser;3. dump tank;4. short-distance distiller;5. product groove;6. residual liquid groove;7. vacuum Machine set system;8. sour spray column;9. activated carbon adsorber.
Specific embodiment
With reference to the accompanying drawings and examples, this utility model is expanded on further.
As shown in figure 1, this utility model is in practical application, add yellow MOCA in distillating still 1, distillating still 1 chuck leads to Enter conduction oil, oil temperature be initially set material can melt temperature, after in kettle, material melts completely, open stirring, water-circulating pump With the vacuum valve being connected to vacuum pump set system 7 on dump tank 3, open the nitrogen valve on distillating still 1, to distillating still 1 simultaneously Inside it is passed through nitrogen, flow-control moisture, free OCA and lower boiling impurity in suitable flow velocity, distillating still 1, pass through After condenser 2 condensation, enter in dump tank 3, when waiting that in kettle, temperature of charge rises to uniform temperature, stop water-circulating pump, open and belong to In the oil circulation vacuum pump of vacuum pump set system 7, redistillation for a period of time, closes the vacuum valve on dump tank 3 and Material valve, Close the nitrogen valve on distillating still 1, set heat conduction oil temperature again, be warming up to temperature of charge uniform temperature in kettle, by nitrogen Decompression kettle adjusts pressure in kettle, then starts the three-level Roots vaccum pump belonging to vacuum pump set system 7, opens short-distance distiller 4 Vacuum valve on motor and connection short-distance distiller 4, opens distillating still 1 bottom valve, so that material is entered by adjusting valve regulating flow Enter in short-distance distiller 4, short-distance distiller 4 has external heat plate and intracavity coldplate, control short-distance distiller 4 heater temperature Degree maintains uniform temperature, and in uniform temperature, system vacuum keeps certain level to the temperature control of internal condensation plate, carries out point Son distillation, product enters in product groove 5, and the high boiling product such as the trimer of generation and polymer enters in residual liquid groove 6, vacuum tail gas High altitude discharge after peracid spray column 8 and activated carbon adsorber 9.The theoretical distillation yield of the white MOCA of gained is 98.11%.Distillation MOCA mass such as following table in front and back:
It should be understood that these embodiments are merely to illustrate this utility model rather than limit scope of the present utility model.This Outward it should be understood that after having read the content of this utility model instruction, those skilled in the art can make each to this utility model Plant and change or change, these equivalent form of values equally fall within the application appended claims limited range.

Claims (8)

1.3,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Including the distillating still being sequentially communicated And short-distance distiller;The gaseous phase outlet of described distillating still has been sequentially communicated condenser and dump tank;Described short-distance distiller also divides It is not communicated with product groove and residual liquid groove;Described dump tank and described short-distance distiller have also been respectively communicated with vacuum pump set system.
2. as claimed in claim 13,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute State vacuum pump set system and be also sequentially communicated sour spray column and activated carbon adsorber.
3. as claimed in claim 13,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute Stating distillating still is the stainless steel cauldron being provided with chuck and agitating device.
4. as claimed in claim 13,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute Stating short-distance distiller is molecular still.
5. as claimed in claim 43,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute State short-distance distiller and be provided with external heat plate and intracavity coldplate.
6. as claimed in claim 13,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute State vacuum pump set system and include vacuum buffer tank, cold-trap surge tank, water circulation vacuum pump, oil circulation vacuum pump and three-level Roots Vacuum pump.
7. as claimed in claim 13,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute Stating condenser is stainless steel condenser, and dump tank is rustless steel dump tank, product groove is stainless steel product groove, residual liquid groove is stainless Steel residual liquid groove.
8. as claimed in claim 23,3 '-two chloro- 4,4 '-diaminodiphenyl-methane purifying plant it is characterised in that:Institute Stating sour spray column is polypropylene antacid spray column, and activated carbon adsorber is polypropylene preparing active carbon adsorption tower.
CN201620903622.XU 2016-08-17 2016-08-17 3, 3' dichloro 4, 4' diamino diphenyl methane device of purifing Active CN205925041U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240686A (en) * 2019-04-29 2019-09-17 山西科灜科技有限公司 A kind of high-performance high-hard, transparent polyurethane elastomer and preparation method thereof
CN111995725A (en) * 2020-09-07 2020-11-27 江苏湘园化工有限公司 Environment-friendly liquid polyurethane curing agent and application method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240686A (en) * 2019-04-29 2019-09-17 山西科灜科技有限公司 A kind of high-performance high-hard, transparent polyurethane elastomer and preparation method thereof
CN111995725A (en) * 2020-09-07 2020-11-27 江苏湘园化工有限公司 Environment-friendly liquid polyurethane curing agent and application method thereof
CN111995725B (en) * 2020-09-07 2022-02-11 江苏湘园化工有限公司 Environment-friendly liquid polyurethane curing agent and application method thereof

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Address after: 262737 Weifang Binhai Economic Development Zone, the Yellow River, West Street, No. 06933, No.

Patentee after: Shandong Chong Shunxin Mstar Technology Ltd

Address before: 262737 Weifang Binhai Economic Development Zone, the Yellow River, West Street, No. 06933, No.

Patentee before: Shandong Chongshun Chemical Co., Ltd.