CN105175287A - Pilot plant for producing ADC foaming agent by oxydol process - Google Patents
Pilot plant for producing ADC foaming agent by oxydol process Download PDFInfo
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- CN105175287A CN105175287A CN201510591089.8A CN201510591089A CN105175287A CN 105175287 A CN105175287 A CN 105175287A CN 201510591089 A CN201510591089 A CN 201510591089A CN 105175287 A CN105175287 A CN 105175287A
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Abstract
The invention provides a pilot plant for producing an ADC foaming agent by an oxydol process, which comprises a reaction system, a vacuum filtration system, a mother solution concentration system, a bromine absorption system, a tail gas treatment system, and pipelines and valves connected with various devices, wherein a reaction kettle contains a stirring paddle, and the material is fed into the reaction kettle from an oxydol storage tank through an oxydol measuring pump; the bottom of the reaction kettle is connected with a vacuum filtration tank and a mother solution tank; the mother solution enters a rectification tower through a mother solution pump, and the concentrated mother solution can be reutilized; the upper end of the reaction kettle is connected with an air compressor and a bromine absorption tower; the bromine absorption tower is connected with an absorption tower circulating pump; the upper end of the reaction kettle is also connected with an anti-overflow tank; and the anti-overflow tank is connected with a tail gas absorption tower, a tail gas tower circulating pump and a negative pressure blower. The pilot plant can effectively solve the problem of recovery of the mother solution and bromine catalyst in the oxydol process for producing the ADC foaming agent, reduce the raw material consumption for pilot plant tests and avoid the problem of treatment of three wastes, thereby providing technical supports for industrial production.
Description
Technical field
The invention belongs to field of chemical equipment, be specifically related to a kind of peroxide passivation and produce ADC whipping agent pilot plant.
Background technology
At present, chlorine method is generally adopted to produce ADC whipping agent, its technical maturity, with low cost, but reaction end is not easy to judge, the a large amount of dilute hydrochloric acid of by-product simultaneously, environmental stress is large, therefore, people start to pay close attention to more clean hydrazo-dicarbonamide oxidation and produce ADC whipping agent technique, the reduzate of hydrogen peroxide is water, and catalyzer and mother liquor can recycles, meet the theory of Green Chemistry.But current peroxide passivation is produced ADC whipping agent and mainly concentrated on the laboratory lab scale stage, seldom consider the recycling problem of catalyzer and mother liquor, University of Fuzhou has carried out pilot scale research, does not still design the recycle device of catalyzer bromine.
Summary of the invention
Object of the present invention is just in order to overcome the deficiency of above-mentioned technology, and provide a kind of peroxide passivation to produce ADC whipping agent pilot plant, set up the system of practicable mother liquor and catalyst recycling, reduce pilot scale raw material consumption, prevent three-protection design problem, thus provide technical support for suitability for industrialized production.
The object of the invention is to have come by following technical solution.This peroxide passivation produces ADC whipping agent pilot plant, comprise reactive system, suction filtration system, mother liquor upgrading system, bromine absorption system, exhaust treatment system, and each equipment be connected pipeline and valve, reactor contains stirring rake, reinforced to reactor from hydrogen peroxide storage tank by hydrogen peroxide volume pump; Connect suction filtration tank and mother liquor tank bottom reactor, mother liquor enters rectifying tower by mother liquor pump, the mother liquor recycling after concentrate; The upper end of reactor connects air compressor and bromine absorption tower, bromine absorption tower connects absorption tower recycle pump; Reactor upper end also connects anti-overflow groove, and anti-overflow groove connects tail gas absorber, tail gas tower recycle pump and negative-pressure air fan.
Hydrogen peroxide concentration in described hydrogen peroxide storage tank is 27.5%, 35% or 50%.
In described bromine absorption tower, absorption liquid is the mineral acid suspension of hydrazo-dicarbonamide.
Mineral acid in the mineral acid suspension of described hydrazo-dicarbonamide is one or more in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid.
Beneficial effect of the present invention is: the present invention effectively can solve the recovery problem that peroxide passivation produces mother liquor and bromine catalyst in ADC whipping agent, reduces pilot scale raw material consumption, prevents three-protection design problem, thus provides technical support for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
In figure, 1 is reactor; 2 is stirring rake; 3 is hydrogen peroxide volume pump; 4 is hydrogen peroxide storage tank; 5 is suction filtration tank; 6 is mother liquor tank; 7 is mother liquor pump; 8 is rectifying tower; 9 is air compressor; 10 is bromine absorption tower; 11 is absorption tower recycle pump; 12 is anti-overflow groove; 13 is tail gas absorber; 14 is tail gas tower recycle pump; 15 is negative-pressure air fan.
Embodiment
Below by embodiment, the present invention is further elaborated, and help is understood the present invention by embodiment better, but the present invention is not limited only to following embodiment.
As shown in Figure 1, this peroxide passivation produces ADC whipping agent pilot plant, comprise reactive system, suction filtration system, mother liquor upgrading system, bromine absorption system, exhaust treatment system, and each equipment be connected pipeline and valve, it is characterized in that: reactor 1 is containing stirring rake 2, reinforced to reactor 1 from hydrogen peroxide storage tank 4 by hydrogen peroxide volume pump 3; Connect suction filtration tank 5 and mother liquor tank 6 bottom reactor 1, mother liquor enters rectifying tower 8 by mother liquor pump 7, the mother liquor recycling after concentrate; The upper end of reactor 1 connects air compressor 9 and bromine absorption tower 10, bromine absorption tower 10 connects absorption tower recycle pump 11; Reactor 1 upper end also connects anti-overflow groove 12, and anti-overflow groove 12 connects tail gas absorber 13, tail gas tower recycle pump 14 and negative-pressure air fan 15.The mother liquor upgrading system of this pilot plant can mineral acid in efficient recovery mother liquor, and recycling, reduces the consumption of raw material, prevent spent acid contaminate environment.Bromine absorption portion effectively can judge reaction end, and absorb by the raw material slip configured the bromine simple substance bloated, convert it into bromide anion, the slip after absorption is squeezed in reactor.
Hydrogen peroxide concentration in described hydrogen peroxide storage tank 4 is 27.5%, 35% or 50%.
In described bromine absorption tower 10, absorption liquid is the mineral acid suspension of hydrazo-dicarbonamide.
Mineral acid in the mineral acid suspension of described hydrazo-dicarbonamide is one or more in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid.
The structural representation of pilot scale synthesizer designed according to this invention, during operation, first check reactor 1, close bottom valve, add water, sulfuric acid, hydrazo-dicarbonamide, Sodium Bromide respectively, be configured to the mineral acid suspension of hydrazo-dicarbonamide, open stirring arm 2, keep absorption tower recycle pump 11, tail gas tower recycle pump 14 and negative-pressure air fan 15 to be in opened condition, make reactor 1 keep tiny structure, then open hydrogen peroxide volume pump 3, control reaction flow velocity and temperature of reaction.After reaction terminates, open air compressor 9, purged by the bromine in reactor 1 and absorb to bromine absorption tower 10, the suspension after absorption can be used as the batching of next still.After purging, open bottom valve, reaction mixture is put into suction filtration tank 5, suction filtration washing leaching cake, dry, be ADC whipping agent product, filtrated stock enters mother liquor tank 6, sends into rectifying tower 8 by mother liquor pump 7, and the mother liquor after rectifying concentrate can be used as reactor batching.
Finally, it should be pointed out that above example is only the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to above-mentioned example, can also have many distortion, all distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, and all should think protection scope of the present invention.
Claims (4)
1. a peroxide passivation produces ADC whipping agent pilot plant, comprise reactive system, suction filtration system, mother liquor upgrading system, bromine absorption system, exhaust treatment system, and each equipment be connected pipeline and valve, it is characterized in that: reactor (1) is containing stirring rake (2), reinforced to reactor (1) from hydrogen peroxide storage tank (4) by hydrogen peroxide volume pump (3); Reactor (1) bottom connects suction filtration tank (5) and mother liquor tank (6), and mother liquor enters rectifying tower (8) by mother liquor pump (7), the mother liquor recycling after concentrate; The upper end of reactor (1) connects air compressor (9) and bromine absorption tower (10), and bromine absorption tower (10) are upper connects absorption tower recycle pump (11); Reactor (1) upper end also connects anti-overflow groove (12), and anti-overflow groove (12) connects tail gas absorber (13), tail gas tower recycle pump (14) and negative-pressure air fan (15).
2. peroxide passivation according to claim 1 produces ADC whipping agent pilot plant, it is characterized in that: the hydrogen peroxide concentration in described hydrogen peroxide storage tank (4) is 27.5%, 35% or 50%.
3. peroxide passivation according to claim 1 produces ADC whipping agent pilot plant, it is characterized in that: in described bromine absorption tower (10), absorption liquid is the mineral acid suspension of hydrazo-dicarbonamide.
4. peroxide passivation according to claim 3 produces ADC whipping agent pilot plant, it is characterized in that: the mineral acid in the mineral acid suspension of described hydrazo-dicarbonamide is one or more in acetic acid, hydrochloric acid, sulfuric acid or phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510591089.8A CN105175287B (en) | 2015-09-17 | 2015-09-17 | Peroxide passivation produces ADC foaming agent pilot-plants |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510591089.8A CN105175287B (en) | 2015-09-17 | 2015-09-17 | Peroxide passivation produces ADC foaming agent pilot-plants |
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| CN105175287A true CN105175287A (en) | 2015-12-23 |
| CN105175287B CN105175287B (en) | 2017-10-31 |
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Cited By (1)
| 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 |
Citations (5)
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|---|---|---|---|---|
| US3876622A (en) * | 1972-08-24 | 1975-04-08 | Eiwa Chemical Ind Company Limi | Process for the preparation of azodicarbonamides modified with metallic compounds |
| US4088643A (en) * | 1975-10-30 | 1978-05-09 | Bayer Aktiengesellschaft | Process for the production of azodicarbonamide |
| CN102335543A (en) * | 2011-08-26 | 2012-02-01 | 莱州诚源盐化有限公司 | Device and method for recovering tail gas 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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2015
- 2015-09-17 CN CN201510591089.8A patent/CN105175287B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3876622A (en) * | 1972-08-24 | 1975-04-08 | Eiwa Chemical Ind Company Limi | Process for the preparation of azodicarbonamides modified with metallic compounds |
| US4088643A (en) * | 1975-10-30 | 1978-05-09 | Bayer Aktiengesellschaft | Process for the production of azodicarbonamide |
| CN102335543A (en) * | 2011-08-26 | 2012-02-01 | 莱州诚源盐化有限公司 | Device and method for recovering tail gas 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 |
Non-Patent Citations (4)
| Title |
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| GALLARD H ET AL: "Kinetic modellling of Fe(Ⅲ)/H2O2 oxidation reactions in dilute aqueous solution using atrazine as a model organic compound", 《WATER RES》 * |
| 施敏明: "ADC发泡剂生产中氧化新工艺的研究——过氧化氢氧化法", 《氯碱工业》 * |
| 陈世豪: "过氧化氢氧化法制偶氮二甲酰胺工艺的研究", 《中国氯碱》 * |
| 陈敏: "过氧化氢氧化法制备发泡剂ADC的研究及其工业化", 《中国优秀硕士学位论文全文数据库——工程科技I辑》 * |
Cited By (1)
| 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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