CN104529002B - Hexamethylenamine produces the recycling treatment process of waste water - Google Patents
Hexamethylenamine produces the recycling treatment process of waste water Download PDFInfo
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- CN104529002B CN104529002B CN201410819212.2A CN201410819212A CN104529002B CN 104529002 B CN104529002 B CN 104529002B CN 201410819212 A CN201410819212 A CN 201410819212A CN 104529002 B CN104529002 B CN 104529002B
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Abstract
The present invention relates to hexamethylenamine production field, particularly relate to the recycling treatment process producing waste water of hexamethylenamine.Based on the research that hexamethylenamine is produced problem existing in waste water, the present inventor provides a kind of hexamethylenamine to produce the recycling treatment process of waste water, the hexamethylenamine in waste water is produced by membrance concentration technique efficient recovery hexamethylenamine, the rejection of hexamethylenamine is reached more than 99%, achieve the resource recycling of hexamethylenamine, improve the yield of hexamethylenamine, decrease resource loss, increase the benefit for enterprise.
Description
Technical field
The present invention relates to hexamethylenamine production field, particularly relate to the recycling treatment process producing waste water of hexamethylenamine.
Background technology
Hexamethylenamine, formal name used at school hexamethylenetetramine is a kind of important chemical products.It can be used as the firming agent of bakelite, the firming agent of aminoplast, the accelerator of the vulcanization of rubber, is all widely used at weaving, food processing, medicine, agricultural, electrolytic industry, analytical chemistry etc..
Hexamethylenamine produces waste water and is primarily referred to as the mother solution in the production process of hexamethylenamine, wherein contains the multiple pollutants such as hexamethylenamine, formaldehyde, methanol and ammonia nitrogen.
Owing to hexamethylenamine produces COD index height in waste water, currently in order to realize discharge standard, enterprise must adopt the advanced oxidation means of Fenton oxidation, catalytic oxidation and other high costs, thus adding the environmental protection treatment cost of enterprise.And due to needs oxidation processes repeatedly, wastewater treatment result is difficult to stably reaching standard, thus results in current hexamethylenamine and produce a process difficult problem for waste water.
Summary of the invention
Producing waste water for current hexamethylenamine to be difficult to process problem up to standard, urotropine wastewater has been carried out more deep research and analysis by the present inventor, it has been found that the major influence factors of its COD index is the hexamethylenamine in production waste water and formaldehyde components.Wherein the content of hexamethylenamine is 1% ~ 2.5%, is difficult to recycle, be difficult to again rationally convert discharge simultaneously during process, thus causing a large amount of hexamethylenamine to run off, production cost increases, and produces waste water simultaneously and is difficult to process, and stably reaching standard discharges.
Based on the research that hexamethylenamine produces problem existing in waste water, the present inventor provides a kind of hexamethylenamine to produce the recycling treatment process of waste water, mainly comprises the steps that
(1) urotropine wastewater is removed float therein, colloidal impurity through filter；
(2) by the ultrafilter membrane ultrafiltration that free from admixture urotropine wastewater via hole diameter is 0.01-0.02 μm after filtration, operation pressure is 2.0-6.0Mpa；
(3) urotropine wastewater by ultrafilter membrane is taken, combine membrane stack combination through nanofiltration and reverse osmosis membrane assembly to retain, operation pressure is 2.0 ~ 6.0Mpa, nanofiltration membrane component permeate enters reverse osmosis membrane assembly, reverse osmosis membrane assembly trapped fluid is back to ultrafilter membrane water inlet end, described NF membrane aperture is 1 ~ 2nm, and molecular cut off is 50-500 dalton, and described reverse osmosis membrane aperture is 0.5-1nm；
(4) nanofiltration membrane component trapped fluid is carried out hexamethylenamine content detection, and reuse is to hexamethylenamine workshop；
(5) hexamethylenamine of reverse osmosis membrane assembly permeate with high temperature is produced waste water and carry out heat exchange by heat exchanger, it is warming up to 50-60 DEG C, and in permeate, adds Calx, regulate the pH to 8 ~ 14 of permeate, then filtrate is heated to 70 ~ 90 DEG C, stir and fully react for 30-60 minute.
(6) will except after formaldehyde reaction solution carry out solid-liquid separation, collect mud and formaldehydeless supernatant respectively, supernatant liquid gives next step wastewater treatment equipment to be further processed.
Preferably, described step (2), (3) filtration all 20 ~ 50 DEG C of operations.
It is further preferable that step (3) is 20 ~ 30 DEG C of operations.
Meanwhile, we are it is further preferred that in step (3), NF membrane is molecular cut off is the daltonian NF membrane of 100-200.
Meanwhile, we it is further disclosed that preferably, and in described step (5), pH is 10 ~ 12.
It is further preferable that Heat preservation 10 ~ 30 minutes in step (5).
In order to better implement the present invention, we further disclose in step (1) described filter is one or several in more medium filter, active carbon filter, accurate filter.
The beneficial effects of the present invention is:
(1) present invention produces the hexamethylenamine in waste water by membrance concentration technique efficient recovery hexamethylenamine, the rejection of hexamethylenamine is reached more than 99%, it is achieved that the resource recycling of hexamethylenamine, improve the yield of hexamethylenamine, decrease resource loss, increase the benefit for enterprise.
(2) present invention reclaims the hexamethylenamine in waste water by membrance concentration technique, it is achieved while resource recycling, greatly reduce the COD in waste water, and the advanced treating producing waste water for hexamethylenamine lightens the load.
(3) present invention adopts lime method to remove hexamethylenamine and produces the formaldehyde in waste water, and formaldehyde clearance reaches more than 99%, effectively reduces hexamethylenamine and produces the bio-toxicity of waste water, solves hexamethylenamine production waste water and is difficult to a difficult problem for biochemical treatment.
Adopt technical scheme disclosed in this invention, it is possible to achieve the recycling of resource, when effectively reducing formaldehyde in waste water and hexamethylenamine content, comprehensively recyle hexamethylenamine, reduce the wasting of resources.And processing method disclosed by the invention, cost is low, simple to operate, is suitable for industrialization large-scale popularization.
Detailed description of the invention
In order to be more fully understood that the present invention, below we the present invention will be further elaborated in conjunction with the embodiments.
Embodiment 1
Collect hexamethylenamine and produce waste water, carry out recycling treatment process according to following steps:
(1) urotropine wastewater is sequentially passed through the visible foreign such as more medium filter, active carbon filter, accurate filter filtration removal float therein, colloidal impurity；
(2) by the ultrafilter membrane ultrafiltration that free from admixture urotropine wastewater via hole diameter is 0.01-0.02 μm after filtration, operation pressure is 2.0-6.0Mpa, and operation temperature is at 20 ~ 50 DEG C；
(3) urotropine wastewater by ultrafilter membrane is taken, combine membrane stack combination through nanofiltration and reverse osmosis membrane assembly to retain, NF membrane aperture is 1 ~ 2nm, molecular cut off is 50-500 dalton,, operation pressure is 2.0 ~ 6.0Mpa, and nanofiltration membrane component permeate enters reverse osmosis membrane assembly, reverse osmosis membrane assembly trapped fluid is back to ultrafilter membrane water inlet end, and reverse osmosis membrane aperture is 0.5-1nm；
(4) nanofiltration membrane component trapped fluid is carried out hexamethylenamine content detection, and reuse is to hexamethylenamine workshop；The recovery rejection of hexamethylenamine reaches more than 99% after testing；
(5) hexamethylenamine of reverse osmosis membrane assembly permeate with high temperature is produced waste water and carry out heat exchange by heat exchanger, it is warming up to 50-60 DEG C, and in permeate, adds Calx, regulate the pH to 8 ~ 14 of permeate, then filtrate is heated to 70 ~ 90 DEG C, stir and fully react for 30-60 minute.
(6) will except after formaldehyde reaction solution carry out solid-liquid separation, collect mud and formaldehydeless supernatant respectively, supernatant liquid gives next step wastewater treatment equipment to be further processed.
Supernatant can also pass through Sewage advanced treatment further, thus conforming better to pollutant emission index.
Embodiment 2
Collect hexamethylenamine and produce waste water, carry out recycling treatment process according to following steps:
Certain factory's hexamethylenamine produces the former water of waste water
(1) urotropine wastewater is sequentially passed through the visible foreign such as more medium filter, active carbon filter, accurate filter filtration removal float therein, colloidal impurity；
(2) by the ultrafilter membrane ultrafiltration that free from admixture urotropine wastewater via hole diameter is 0.01 μm after filtration, operation pressure is 4.0Mpa, and operation temperature is at 20 DEG C；
(3) urotropine wastewater by ultrafilter membrane is taken, combine membrane stack combination through nanofiltration and reverse osmosis membrane assembly to retain, NF membrane aperture is 1nm, molecular cut off is 100 dalton,, operation pressure is 4.0Mpa, and nanofiltration membrane component permeate enters reverse osmosis membrane assembly, reverse osmosis membrane assembly trapped fluid is back to ultrafilter membrane water inlet end, and reverse osmosis membrane aperture is 0.5nm；
(4) nanofiltration membrane component trapped fluid is carried out hexamethylenamine content detection, and reuse is to hexamethylenamine workshop；The recovery rejection of hexamethylenamine reaches more than 99% after testing；
(5) hexamethylenamine of reverse osmosis membrane assembly permeate with high temperature is produced waste water and carry out heat exchange by heat exchanger, it is warming up to 50 DEG C, and in permeate, adds Calx, regulate the pH to 12 of permeate, then filtrate is heated to 70 DEG C, stir and fully react for 30 minutes.
(6) will except after formaldehyde reaction solution carry out solid-liquid separation, collect mud and formaldehydeless supernatant respectively, supernatant liquid gives next step wastewater treatment equipment to be further processed.
Supernatant can also pass through Sewage advanced treatment further, thus conforming better to pollutant emission index.
Embodiment 3
Collect hexamethylenamine and produce waste water, carry out recycling treatment process according to following steps:
(1) urotropine wastewater is sequentially passed through the visible foreign such as more medium filter, active carbon filter, accurate filter filtration removal float therein, colloidal impurity；
(2) by the ultrafilter membrane ultrafiltration that free from admixture urotropine wastewater via hole diameter is 0.02 μm after filtration, operation pressure is 4.5Mpa, and operation temperature is at 25 DEG C；
(3) urotropine wastewater by ultrafilter membrane is taken, combine membrane stack combination through nanofiltration and reverse osmosis membrane assembly to retain, NF membrane aperture is 1nm, molecular cut off is 100 dalton,, operation pressure is 4.5Mpa, and nanofiltration membrane component permeate enters reverse osmosis membrane assembly, reverse osmosis membrane assembly trapped fluid is back to ultrafilter membrane water inlet end, and reverse osmosis membrane aperture is 0.5nm；
(4) nanofiltration membrane component trapped fluid is carried out hexamethylenamine content detection, and reuse is to hexamethylenamine workshop；The recovery rejection of hexamethylenamine reaches more than 99% after testing；
(5) hexamethylenamine of reverse osmosis membrane assembly permeate with high temperature is produced waste water and carry out heat exchange by heat exchanger, it is warming up to 50 DEG C, and in permeate, adds Calx, regulate the pH to 8 ~ 14 of permeate, then filtrate is heated to 80 DEG C, stir and fully react for 40 minutes.
(6) will except after formaldehyde reaction solution carry out solid-liquid separation, collect mud and formaldehydeless supernatant respectively, supernatant liquid gives next step wastewater treatment equipment to be further processed.
Supernatant can also pass through Sewage advanced treatment further, thus conforming better to pollutant emission index.
Claims (6)
1. hexamethylenamine produces a recycling treatment process for waste water, it is characterized in that, mainly comprises the steps that
(1) urotropine wastewater is removed float therein, colloidal impurity through filter；
(2) by the ultrafilter membrane ultrafiltration that free from admixture urotropine wastewater via hole diameter is 0.01-0.02 μm after filtration, operation pressure is 2.0-6.0Mpa；
(3) urotropine wastewater by ultrafilter membrane is taken, it is 1 ~ 2nm through aperture, molecular cut off be the daltonian nanofiltration of 50-500 and reverse osmosis membrane assembly combination membrane stack combination retain, operation pressure is 2.0 ~ 6.0MPa, and urotropine wastewater is divided into trapped fluid and permeate two parts；
(4) nanofiltration membrane component trapped fluid is carried out hexamethylenamine content detection, and reuse is to hexamethylenamine workshop；
(5) will transmit through liquid and be warming up to 50-60 DEG C, and in permeate, add Calx, regulate the pH to 8 ~ 12 of permeate, stir and fully react for 30-60 minute,
(6) will by step (5) except after formaldehyde reaction solution carry out precipitate and separate, collect mud and formaldehydeless supernatant respectively, supernatant gives next step wastewater treatment equipment to be further processed.
2. hexamethylenamine according to claim 1 produce waste water recycling treatment process, it is characterized in that, described step (2), (3) filtration all 20 ~ 50 DEG C of operations.
3. hexamethylenamine according to claim 2 produces the recycling treatment process of waste water, it is characterized in that, described step (3) is 20 ~ 30 DEG C of operations.
4. hexamethylenamine as claimed in any of claims 1 to 3 produces the recycling treatment process of waste water, it is characterized in that, in described step (3), NF membrane is molecular cut off is the daltonian NF membrane of 100-200；In described step (5), pH is 10 ~ 12；
Heat preservation 10 ~ 30 minutes after being warming up to 50-60 DEG C in step (5).
5. hexamethylenamine according to claim 1 produces the recycling treatment process of waste water, it is characterized in that, the filter described in step (1) is one or several in more medium filter, active carbon filter, accurate filter.
6. hexamethylenamine according to claim 1 produces the recycling treatment process of waste water, it is characterized in that, in described step (5), the hexamethylenamine of permeate and high temperature produces waste water and carries out heat exchange by heat exchanger, is warming up to 50 ~ 60 DEG C.
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