CN105175287B - Peroxide passivation produces ADC foaming agent pilot-plants - Google Patents

Peroxide passivation produces ADC foaming agent pilot-plants Download PDF

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Publication number
CN105175287B
CN105175287B CN201510591089.8A CN201510591089A CN105175287B CN 105175287 B CN105175287 B CN 105175287B CN 201510591089 A CN201510591089 A CN 201510591089A CN 105175287 B CN105175287 B CN 105175287B
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China
Prior art keywords
mother liquor
reactor
bromine
plants
foaming agent
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CN201510591089.8A
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CN105175287A (en
Inventor
陈海贤
徐智锋
魏增
徐朝辉
寿元军
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HANGZHOU HI-TECH FINE CHEMICAL Co Ltd
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HANGZHOU HI-TECH FINE CHEMICAL Co Ltd
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Abstract

ADC foaming agent pilot-plants are produced the invention provides a kind of peroxide passivation, including reaction system, suction filtration system, mother liquor upgrading system, bromine absorption system, exhaust treatment system, and each equipment connected pipeline and valve, reactor contains agitating paddle, is fed by hydrogen peroxide measuring pump from dioxygen water storage tank into reactor;Reactor bottom connects suction filtration tank and mother liquor tank, and mother liquor enters the mother liquor after rectifying column, concentrate by mother liquor pump and reused;Absorption tower circulating pump is connected on the upper end connection air compressor of reactor and bromine absorption tower, bromine absorption tower;Reactor upper end is also connected with anti-overflow groove, anti-overflow groove connection tail gas absorber, tail gas tower circulating pump and negative-pressure air fan.Beneficial effects of the present invention are:The present invention can effectively solve the problems, such as the recovery of mother liquor and bromine catalyst in peroxide passivation production ADC foaming agents, reduce pilot scale consumption of raw materials, three-protection design problem is prevented, so as to provide technical support for industrialized production.

Description

Peroxide passivation produces ADC foaming agent pilot-plants
Technical field
The invention belongs to field of chemical equipment, and in particular to a kind of peroxide passivation produces ADC foaming agent pilot-plants.
Background technology
At present, generally using chlorine method production ADC foaming agents, its technical maturity is with low cost, but reaction end is not allowed Easily judge, while a large amount of watery hydrochloric acid of by-product, environmental pressure is big, therefore, people begin to focus on the biruea oxidation production more cleaned ADC foaming agent techniques, the reduzate of hydrogen peroxide is water, and catalyst and mother liquor can be recycled, and meet Green Chemistry Theory.But, current peroxide passivation production ADC foaming agents are concentrated mainly on the laboratory lab scale stage, seldom consider catalyst and The recycling problem of mother liquor, University of Fuzhou has carried out pilot scale research, does not still design the recycling dress of catalyst bromine Put.
The content of the invention
The purpose of the present invention is precisely in order to overcome the shortcomings of above-mentioned technology, and provide a kind of peroxide passivation production ADC foaming Agent pilot-plant, sets up the system of practicable mother liquor and catalyst recycling, reduces pilot scale consumption of raw materials, prevents the three wastes Process problem, so as to provide technical support for industrialized production.
The purpose of the present invention is completed by following technical solution.This peroxide passivation produces ADC foaming agent pilot scales Device, including reaction system, suction filtration system, mother liquor upgrading system, bromine absorption system, exhaust treatment system, and each equipment phase Pipeline and valve even, reactor contains agitating paddle, is fed by hydrogen peroxide measuring pump from dioxygen water storage tank into reactor;Instead Bottom portion is answered to connect suction filtration tank and mother liquor tank, mother liquor enters the mother liquor after rectifying column, concentrate by mother liquor pump and reused;Reaction Absorption tower circulating pump is connected on the upper end connection air compressor of kettle and bromine absorption tower, bromine absorption tower;Reactor upper end is also connected with Anti-overflow groove, anti-overflow groove connection tail gas absorber, tail gas tower circulating pump and negative-pressure air fan.
Hydrogen peroxide concentration in described dioxygen water storage tank is 27.5%, 35% or 50%.
Absorbing liquid is the inorganic acid suspension of biruea in described bromine absorption tower.
Inorganic acid in the inorganic acid suspension of described biruea is one kind in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid Or it is several.
Beneficial effects of the present invention are:The present invention can effectively solve mother liquor and bromine in peroxide passivation production ADC foaming agents The recovery problem of catalyst, reduces pilot scale consumption of raw materials, three-protection design problem is prevented, so as to provide technology branch for industrialized production Hold.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention.
1 is reactor in figure;2 be agitating paddle;3 be hydrogen peroxide measuring pump;4 be dioxygen water storage tank;5 be suction filtration tank;6 be mother Liquid bath;7 be mother liquor pump;8 be rectifying column;9 be air compressor;10 be bromine absorption tower;11 be absorption tower circulating pump;12 be anti-overflow Groove;13 be tail gas absorber;14 be tail gas tower circulating pump;15 be negative-pressure air fan.
Embodiment
Below by embodiment, the present invention is further elaborated, and embodiment will facilitate a better understanding of this hair It is bright, but the present invention is not limited only to following embodiments.
As shown in figure 1, this peroxide passivation production ADC foaming agent pilot-plants, including reaction system, suction filtration system, mother Liquid upgrading system, bromine absorption system, exhaust treatment system, and each equipment connected pipeline and valve, it is characterised in that:Reaction Kettle 1 contains agitating paddle 2, is fed by hydrogen peroxide measuring pump 3 from dioxygen water storage tank 4 into reactor 1;The bottom of reactor 1 is connected Suction filtration tank 5 and mother liquor tank 6, the mother liquor recycling that mother liquor is entered after rectifying column 8, concentrate by mother liquor pump 7;Reactor 1 it is upper Absorption tower circulating pump 11 is connected on end connection air compressor 9 and bromine absorption tower 10, bromine absorption tower 10;The upper end of reactor 1 also connects Take over control excessive groove 12, the anti-overflow connection of groove 12 tail gas absorber 13, tail gas tower circulating pump 14 and negative-pressure air fan 15.The mother of the pilot-plant Liquid upgrading system can effectively reclaim the inorganic acid in mother liquor, recycling, reduce the consumption of raw material, prevent spent acid from polluting environment. Bromine, which absorbs part, can effectively judge reaction end, and the bromine simple substance of bulging is absorbed by the raw material slurry configured, is converted it into Bromide ion, the slurry after absorption is squeezed into reactor.
Hydrogen peroxide concentration in described dioxygen water storage tank 4 is 27.5%, 35% or 50%.
Absorbing liquid is the inorganic acid suspension of biruea in described bromine absorption tower 10.
Inorganic acid in the inorganic acid suspension of described biruea is one kind in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid Or it is several.
The structural representation of pilot scale synthesizer, during operation, first checks reactor 1, closes bottom designed according to this invention Portion's valve, is separately added into water, sulfuric acid, biruea, sodium bromide, is configured to the inorganic acid suspension of biruea, opens stirring slurry 2, Keep absorption tower circulating pump 11, tail gas tower circulating pump 14 and negative-pressure air fan 15 to be in opening, reactor 1 is kept micro- negative Pressure, is then turned on hydrogen peroxide measuring pump 3, control reaction flow velocity and reaction temperature.After reaction terminates, air compressor 9 is opened, will Bromine in reactor 1, which is purged to bromine absorption tower 10, to be absorbed, the suspension after absorption can as next kettle dispensing.Purging is finished Afterwards, bottom valve is opened, reactant mixture suction filtration tank 5 is put into, suction filtration simultaneously washs filter cake, dried, as ADC foaming agents product, mistake Filter mother liquor and enter mother liquor tank 6, the mother liquor sent into by mother liquor pump 7 after rectifying column 8, rectifying concentrate can be used as reactor dispensing.
Finally it is pointed out that above example is only the more representational example of the present invention.Obviously, technical side of the invention Case is not limited to examples detailed above, can also there is many deformations, and one of ordinary skill in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (4)

1. a kind of peroxide passivation produces ADC foaming agent pilot-plants, including reaction system, suction filtration system, mother liquor upgrading system, bromine Absorption system, exhaust treatment system, and each equipment connected pipeline and valve, it is characterised in that:Reactor (1) contains stirring Oar (2), feeds by the way that hydrogen peroxide measuring pump (3) is middle from dioxygen water storage tank (4) to reactor (1);The series connection of reactor (1) bottom connects Suction filtration tank (5) and mother liquor tank (6) are connect, mother liquor pump (7) is connected with mother liquor tank (6), and mother liquor enters rectifying column by mother liquor pump (7) (8), the mother liquor recycling after concentrate;The upper end of reactor (1) is connected in parallel air compressor (9) and bromine absorption tower (10), Absorption tower circulating pump (11) is connected on bromine absorption tower (10);Reactor (1) upper end is also connected with anti-overflow groove (12), and anti-overflow groove (12) is even Tail gas absorber (13) is connect, tail gas absorber (13) is connected with tail gas tower circulating pump (14), negative-pressure air fan (15) respectively.
2. peroxide passivation according to claim 1 produces ADC foaming agent pilot-plants, it is characterised in that:Described dioxygen Hydrogen peroxide concentration in water storage tank (4) is 27.5%, 35% or 50%.
3. peroxide passivation according to claim 1 produces ADC foaming agent pilot-plants, it is characterised in that:Described bromine is inhaled Receive the inorganic acid suspension that absorbing liquid in tower (10) is biruea.
4. peroxide passivation according to claim 3 produces ADC foaming agent pilot-plants, it is characterised in that:Described di- Inorganic acid in the inorganic acid suspension of urea is the one or more in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid.
CN201510591089.8A 2015-09-17 2015-09-17 Peroxide passivation produces ADC foaming agent pilot-plants Active CN105175287B (en)

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CN105175287B true CN105175287B (en) 2017-10-31

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Publication number Priority date Publication date Assignee Title
CN110790688A (en) * 2019-10-09 2020-02-14 江苏远洋药业股份有限公司 A device for taurine fine work mother liquor purifies

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JPS5037173B2 (en) * 1972-08-24 1975-12-01
DE2548592C3 (en) * 1975-10-30 1979-06-21 Bayer Ag, 5090 Leverkusen Process for the production of azodicarbonamide
CN102335543B (en) * 2011-08-26 2013-08-07 莱州诚源盐化有限公司 Device and method for recovering exhaust in bromine packaging
CN102942508A (en) * 2012-11-13 2013-02-27 杭州海虹精细化工有限公司 Method for continuously producing ADC (azodicarbonamide) foaming agent
CN103058893A (en) * 2013-01-21 2013-04-24 陈世豪 Method for preparing azodicarbonamide by hydrogen peroxide oxidization method

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