CN107233801A - The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid - Google Patents
The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid Download PDFInfo
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- CN107233801A CN107233801A CN201710683139.4A CN201710683139A CN107233801A CN 107233801 A CN107233801 A CN 107233801A CN 201710683139 A CN201710683139 A CN 201710683139A CN 107233801 A CN107233801 A CN 107233801A
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- Prior art keywords
- mpd
- spent acid
- membrane
- phenylene diamine
- acid
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/24—Dialysis ; Membrane extraction
- B01D61/28—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/24—Dialysis ; Membrane extraction
- B01D61/243—Dialysis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/905—Removal of organic impurities
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention discloses a kind of device of m-phenylene diamine (MPD) in UF membrane spent acid, including a diffusion dialysis film device, spent acid entrance, water inlet, regenerated acid outlet and raffinate outlet are respectively equipped with the diffusion dialysis film device；The anion-exchange membrane for being used for separating diffuser casing and dialysing compartment is provided with the diffusion dialysis film device；The anion-exchange membrane is, by will be immersed as the polymer of matrix in film liquid, to form the basement membrane of densification in described matrix surface aggregate, then the basement membrane is immersed into what is obtained in amination liquid through aminating reaction.The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid of the present invention, is that the processing up to standard of waste water successive depths or acid recovery provide guarantee, the sulfuric acid resourcebility isolated is reclaimed, and while waste water is administered, realizes changing waste into resources.
Description
Technical field
The present invention relates to wastewater treating technology field, a kind of device of m-phenylene diamine (MPD) in UF membrane spent acid is particularly related to
And method.
Background technology
M-phenylene diamine (MPD) (m-Phenylenediamine, abbreviation MPD) is a kind of toxic chemical, stimulates eyes and skin.
The material can be absorbed in vivo by sucking its steam through skin and eating, repeatedly or Long Term Contact may cause allergic,
May have an impact to kidney and blood, cause kidney failure and form methamoglobin.It is scattered that m-phenylene diamine (MPD) is widely used in manufacture
Dyestuff, reactive dye and direct dyes and accelerator for cement slurry.It can be produced containing a large amount of isophthalic while m-phenylene diamine (MPD) is produced
The spent acid of diamines, efficient, economic industrialization Processing tecchnics are lacked for this spent acid, chemical enterprise is seriously constrained at this stage
Development, also have great harm for environmental protection.
The content of the invention
In view of defect present in above-mentioned prior art, the purpose of the present invention is to propose to isophthalic two in a kind of UF membrane spent acid
The separation of m-phenylene diamine (MPD) and sulfuric acid in the device and method of amine, the peracid high-COD waste water for solving production m-phenylene diamine (MPD) and producing
Recovery problem.
To achieve these goals, present invention employs following technical scheme：
The device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid, including a diffusion dialysis film device, the diffusion dialysis film dress
Put and be respectively equipped with spent acid entrance, water inlet, regenerated acid outlet and raffinate outlet；Being provided with the diffusion dialysis film device is used for
Separate the anion-exchange membrane of diffuser casing and dialysing compartment；The anion-exchange membrane is by will be immersed as the polymer of matrix
In film liquid, the basement membrane of densification is formed in described matrix surface aggregate, then will be obtained in basement membrane immersion amination liquid through aminating reaction
Arrive.
Further, the polymer is selected from polyphenylene oxide or polysulfones.
Further, it is 0.5 that the film liquid, which includes mol ratio,:100-1:100 reactant and initiator, the reactant
It is 5 including mol ratio:1-10:1 monomer and crosslinking agent.
Further, the monomer is styrene, and the crosslinking agent is divinylbenzene, and the initiator is benzoyl peroxide first
Acyl and azodiisobutyronitrile.
Further, in the aminating reaction, the amination liquid is the front three that Solution percentages concentration is 5%-20%
Amine aqueous solution, amination temperature is 20 DEG C -50 DEG C, and the amination time is 10h-56h.
Further, the regenerated acid outlet and raffinate outlet are in same level height.
A kind of method of m-phenylene diamine (MPD) in UF membrane spent acid, based on m-phenylene diamine (MPD) in any one above-mentioned UF membrane spent acid
Device, comprise the following steps：
Step one：The spent acid progress filtration treatment that m-phenylene diamine (MPD) is produced will be produced；
Step 2：The spent acid after the filtering of same volume and water is taken to be injected respectively from the spent acid entrance and the water inlet
In described device；
Step 3：- 4 hours 1 hour are stood, the solution in described device is reached balance；
Step 4：After diffusion dialysis, from the regenerated acid outlet and the raffinate outlet in respectively obtain recovery acid and
Raffinate containing m-phenylene diamine (MPD).
Further, in the step 2, the flow velocity of the spent acid and water is 5ml/min-20ml/min.
The present invention protrusion effect be：The device and method of m-phenylene diamine (MPD), is used in a kind of UF membrane spent acid of the present invention
Process for producing m-phenylene diamine (MPD) and the peracid high-COD waste water produced, by filtering after pretreatment, with certain flow rate by waste water with originally
Water by being filled with the experimental provision of diffusion dialysis film, is dammed the material with positive charge by anion-exchange membrane simultaneously,
Waste water can be efficiently separated into raffinate and recovery acid, m-phenylene diamine (MPD) is efficiently separated with sulfuric acid, be waste water successive depths place up to standard
Reason or acid recovery, which are provided, to be ensured, the sulfuric acid resourcebility isolated is reclaimed, and while waste water is administered, realizes waste resource
Change.
Brief description of the drawings
Fig. 1 is 1-2 of embodiment of the present invention structural representation；
In figure：Diffusion dialysis film device 1；Spent acid entrance 2；Water inlet 3；Regenerated acid outlet 4；Raffinate outlet 5；Anion is handed over
Change film 6.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.
Embodiment 1
As shown in figure 1, in a kind of UF membrane spent acid of the present embodiment m-phenylene diamine (MPD) device, including diffusion dialysis film device
1, spent acid entrance 2, water inlet 3, regenerated acid outlet 4 and raffinate outlet 5 are respectively equipped with diffusion dialysis film device 1；Regenerated acid goes out
Mouth 4 and raffinate outlet 5 are in same level height.
The anion-exchange membrane 6 for being used for separating diffuser casing and dialysing compartment is provided with diffusion dialysis film device 1；Anion exchange
Film 6 is by being immersed as the polymer of matrix in film liquid, the basement membrane to form densification being polymerize in matrix surface, then basement membrane is soaked
Enter what is obtained in amination liquid through aminating reaction.
Wherein, polymer is selected from polyphenylene oxide or polysulfones.
It is 0.5 that film liquid, which includes mol ratio,:100 reactant and initiator, it is 10 that reactant, which includes mol ratio,:1 monomer
And crosslinking agent.Monomer is styrene, and crosslinking agent is divinylbenzene, and initiator is benzoyl peroxide and azodiisobutyronitrile.
In aminating reaction, the amination liquid is the trimethylamine solution that Solution percentages concentration is 5%, and amination temperature is 20
DEG C, the amination time is 56h.
Embodiment 2
As shown in figure 1, in a kind of UF membrane spent acid of the present embodiment m-phenylene diamine (MPD) device, including diffusion dialysis film device
1, spent acid entrance 2, water inlet 3, regenerated acid outlet 4 and raffinate outlet 5 are respectively equipped with diffusion dialysis film device 1；Regenerated acid goes out
Mouth 4 and raffinate outlet 5 are in same level height.
The anion-exchange membrane 6 for being used for separating diffuser casing and dialysing compartment is provided with diffusion dialysis film device 1；Anion exchange
Film 6 is by being immersed as the polymer of matrix in film liquid, the basement membrane to form densification being polymerize in matrix surface, then basement membrane is soaked
Enter what is obtained in amination liquid through aminating reaction.
Wherein, polymer is selected from polyphenylene oxide or polysulfones.
It is 1 that film liquid, which includes mol ratio,:100 reactant and initiator, it is 5 that reactant, which includes mol ratio,:1 monomer and friendship
Join agent.Monomer is styrene, and crosslinking agent is divinylbenzene, and initiator is benzoyl peroxide and azodiisobutyronitrile.
In aminating reaction, the amination liquid is the trimethylamine solution that Solution percentages concentration is 20%, and amination temperature is
50 DEG C, the amination time is 10h.
Embodiment 3：
The method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid of the present embodiment, a kind of UF membrane spent acid based on embodiment 1
The device of middle m-phenylene diamine (MPD), comprises the following steps：
Step one：By certain dyestuff enterprise produce m-phenylene diamine (MPD) produce spent acid (using calcium carbonate acidity as
603202.6ppm, m-phenylene diamine (MPD) content is 35006.9ppm) carry out filtration treatment, to remove clean suspension therein and
Colloid；
Step 2：Take the spent acid after the filtering of same volume and water respectively from spent acid entrance and water inlet injection device,
The flow velocity of spent acid and water is respectively 18ml/min and 20ml/min；
Step 3：1 hour is stood, the solution in device is reached balance；
Step 4：After diffusion dialysis, respectively obtain recovery acid from regenerated acid outlet and raffinate outlet and contain isophthalic
The raffinate of diamines.
Recovery acid is taken to be measured with raffinate, experimental data is shown in Table 1, it can be seen that, the processing method of the present embodiment is effective
Ground is separated m-phenylene diamine (MPD) with sulfuric acid, and raffinate can carry out extraction and recovery m-phenylene diamine (MPD), and recovery acid can be used as factory's reuse.
Table 1
Embodiment 4：
The method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid of the present embodiment, a kind of UF membrane spent acid based on embodiment 2
The device of middle m-phenylene diamine (MPD), comprises the following steps：
Step one：By certain dyestuff enterprise produce m-phenylene diamine (MPD) produce spent acid (using calcium carbonate acidity as 301205ppm,
M-phenylene diamine (MPD) content is 38945ppm) filtration treatment is carried out, to remove clean suspension and colloid therein；
Step 2：Take the spent acid after the filtering of same volume and water respectively from spent acid entrance and water inlet injection device,
The flow velocity of spent acid and water is respectively 11ml/min and 10ml/min；
Step 3：4 hours are stood, the solution in device is reached balance；
Step 4：After diffusion dialysis, respectively obtain recovery acid from regenerated acid outlet and raffinate outlet and contain isophthalic
The raffinate of diamines.
Recovery acid is taken to be measured with raffinate, experimental data is shown in Table 2, it can be seen that, the processing method of the present embodiment is effective
Ground is separated m-phenylene diamine (MPD) with sulfuric acid, and raffinate can carry out extraction and recovery m-phenylene diamine (MPD), and recovery acid can be used as factory's reuse.
Table 2
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
1. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid, it is characterised in that：Including a diffusion dialysis film device, the diffusion
Spent acid entrance, water inlet, regenerated acid outlet and raffinate outlet are respectively equipped with dialysis film device；In the diffusion dialysis film device
Provided with the anion-exchange membrane for separating diffuser casing and dialysing compartment；The anion-exchange membrane is by will be used as the poly- of matrix
In compound immersion film liquid, the basement membrane of densification is formed in described matrix surface aggregate, then the basement membrane is immersed in amination liquid through amine
Change what reaction was obtained.
2. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 1, it is characterised in that：The polymer
Selected from polyphenylene oxide or polysulfones.
3. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 1, it is characterised in that：The film liquid bag
It is 0.5 to include mol ratio:100-1:100 reactant and initiator, it is 5 that the reactant, which includes mol ratio,:1-10:1 monomer
And crosslinking agent.
4. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 3, it is characterised in that：The monomer is
Styrene, the crosslinking agent is divinylbenzene, and the initiator is benzoyl peroxide and azodiisobutyronitrile.
5. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 1, it is characterised in that：In the amination
In reaction, the amination liquid is the trimethylamine solution that Solution percentages concentration is 5%-20%, and amination temperature is 20 DEG C -50 DEG C,
The amination time is 10h-56h.
6. the device of m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 1, it is characterised in that：The regenerated acid
Outlet and raffinate outlet are in same level height.
7. a kind of method of m-phenylene diamine (MPD) in UF membrane spent acid, based on any one UF membrane spent acid described in claim 1-5
The device of middle m-phenylene diamine (MPD), it is characterised in that comprise the following steps：
Step one：The spent acid progress filtration treatment that m-phenylene diamine (MPD) is produced will be produced；
Step 2：Take the spent acid after the filtering of same volume and water described from the spent acid entrance and water inlet injection respectively
In device；
Step 3：- 4 hours 1 hour are stood, the solution in described device is reached balance；
Step 4：After diffusion dialysis, respectively obtain recovery acid from regenerated acid outlet and raffinate outlet and contain
The raffinate of m-phenylene diamine (MPD).
8. the method for m-phenylene diamine (MPD) in a kind of UF membrane spent acid according to claim 7, it is characterised in that：The step 2
In, the flow velocity of the spent acid and water is 5ml/min-20ml/min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710683139.4A CN107233801A (en) | 2017-08-11 | 2017-08-11 | The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710683139.4A CN107233801A (en) | 2017-08-11 | 2017-08-11 | The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid |
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| CN107233801A true CN107233801A (en) | 2017-10-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710683139.4A Pending CN107233801A (en) | 2017-08-11 | 2017-08-11 | The device and method of m-phenylene diamine (MPD) in a kind of UF membrane spent acid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663547A (en) * | 2012-09-24 | 2014-03-26 | 上海凯鑫分离技术有限公司 | Treatment and recovery process of acid wastewater in titanium dioxide production process |
| WO2015011063A1 (en) * | 2013-07-25 | 2015-01-29 | Fresenius Medical Care Deutschland Gmbh | Method and device for monitoring an extracorporeal blood circuit |
| CN205501001U (en) * | 2016-04-18 | 2016-08-24 | 长兴汇能电源有限公司 | Waste acid recycling utilizes equipment |
| CN106422802A (en) * | 2016-11-12 | 2017-02-22 | 杭州科百特过滤器材有限公司 | Method for preparing homogenous ion exchange membranes |
-
2017
- 2017-08-11 CN CN201710683139.4A patent/CN107233801A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663547A (en) * | 2012-09-24 | 2014-03-26 | 上海凯鑫分离技术有限公司 | Treatment and recovery process of acid wastewater in titanium dioxide production process |
| WO2015011063A1 (en) * | 2013-07-25 | 2015-01-29 | Fresenius Medical Care Deutschland Gmbh | Method and device for monitoring an extracorporeal blood circuit |
| CN205501001U (en) * | 2016-04-18 | 2016-08-24 | 长兴汇能电源有限公司 | Waste acid recycling utilizes equipment |
| CN106422802A (en) * | 2016-11-12 | 2017-02-22 | 杭州科百特过滤器材有限公司 | Method for preparing homogenous ion exchange membranes |
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Application publication date: 20171010 |