CN101992132A - Ion exchange waste water denitrification material and preparation method thereof - Google Patents
Ion exchange waste water denitrification material and preparation method thereof Download PDFInfo
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- CN101992132A CN101992132A CN2010105579597A CN201010557959A CN101992132A CN 101992132 A CN101992132 A CN 101992132A CN 2010105579597 A CN2010105579597 A CN 2010105579597A CN 201010557959 A CN201010557959 A CN 201010557959A CN 101992132 A CN101992132 A CN 101992132A
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Abstract
The invention relates to an ion exchange waste water denitrification material and a preparation method thereof. A segmented copolymer containing a polyolefin acetal chain segment and a polyolefin sodium carboxylate chain segment is prepared from polyolefin alcohol and polyolefin sodium carboxylate which have low polymerization degree, as well as aldehydes, kieselguhr, kaolin, imvite and the like under the action of an initiator. The copolymer has sodium carboxylate groups, can be used as cation exchange resin, and performs the exchange with NH4<+> in waste water;and the roughness of the material can be increased by adding inorganic nanometer powder soil, and the specific surface area is increased to improve the hydrophily and affiliation capacity of microbes. The preparation method comprises the following steps of: dissolving the polyolefin alcohol and the polyolefin sodium carboxylate by using NaSCN solution, adding the initiator for polymerizing, adding a terminator and inorganic nanometer powder, stirring and mixing uniformly to prepare spinning solution, coagulating the spinning solution with inorganic salt solution in coagulating bath to form nascent fibers, performing post processing processes such as drawing, heat setting, acetalation, washing, drying and the like, and weaving to form a specific shape to obtain the required product. The material has the good mechanical strength, hydrophily, microbe affinity and ion exchange performance.
Description
Technical field
The invention belongs to the wastewater treatment field of functional materials, be specifically related to a kind of preparation method of ion-exchange type denitrogenation of waste water functional material.
Background technology
Along with the raising of people's living standard, also more and more higher to the requirement of environmental quality.Since the eighties in 20th century, the many lake and reservoir water bodys of China are tending towards eutrophication and are increasing the weight of trend, as body eutrophication problems such as Taihu Lake, Dian Chi, Guanting reservoirs, the ecosystem and socio-economic development have been constituted very big restriction and influence.The polluted by nitrogen of water quality can bring serious harm to the aquatic animals and plants and the mankind, is necessary to study denitrogenation of waste water material efficiently under the situation of this sternness.
In recent years, in waste water and micro-polluted water process field, biomembrance process has obtained application more and more widely.The core of biomembrance process is a packing technique.Filler affects microbial growth, breeds, comes off and form as microorganism carrier, thereby, the operational effect and the energy consumption of biochemical reaction all there is crucial influence.Filler is by elasticity classification, can be divided into soft, medium-soft, filler such as rigid.What domestic current application was more is elastic filler and combined stuffing etc., but all has not shortcoming such as easy to be filmed, hydrophily difference of microorganism, and therefore developing a kind of novel denitrogenation of waste water filler has very big meaning.
Summary of the invention
The object of the present invention is to provide a kind of possess hydrophily, close microorganism property, ion-exchange type denitrification functions material that intensity is high and preparation method thereof.
The present invention at first uses the pure and mild polyolefinic acid sodium of a certain proportion of polyolefin of dissolution with solvents, initator, dispersant etc., add terminator behind the polymerization certain hour, add one or more nano-powders such as 2～18% diatomite, kaolin, imvite again, and after high-speed stirred mixes it, prepare the spinning solution that possesses certain viscosity, after being spun to as-spun fibre, through being woven into given shape after the procedure of processings such as acetalation processing, obtain finished product again.
The ion-exchange type denitrification functions material that the present invention proposes, described functional material is made up of solvent, polyolefin alcohol, polyolefinic acid sodium, initator, terminator, dispersant and inorganic nanometer powder, by weight percentage:
Solvent 25%～58%,
Polyolefin alcohol 10%～21%,
Polyolefinic acid sodium 10%～21%,
Initator 0.01%～0.8%,
Terminator 0.01%～0.2%,
Dispersant 2%～6%,
All the other are inorganic nanometer powder, and its gross weight satisfies 100%.
Among the present invention, described solvent is NaSCN (Chinese name) solution.
Among the present invention, described initator is azodiisobutyronitrile or potassium peroxydisulfate.
Among the present invention, described reactant polyolefin alcohol is in polyvinyl alcohol or the POLYPROPYLENE GLYCOL one to two kind.
Among the present invention, described reactant polyolefinic acid sodium is in Sodium Polyacrylate or the sodium polymethacrylate one to two kind.
Among the present invention, described terminator is acetic acid or tetrasodium salt of EDTA.
Among the present invention, described dispersant is one to several in lauryl sodium sulfate, neopelex, the dodecyl sodium sulfate.
Among the present invention, described inorganic nanometer powder is one to several in diatomite, kaolin or the imvite.
The ion-exchange type denitrification functions preparation methods that the present invention proposes, concrete steps are:
(1) with dissolution with solvents polyolefin alcohol, polyolefinic acid sodium, initator and dispersant, 60 ℃ ~ 85 ℃ and mixing speed is to carry out polymerisation under 200r/min～600r/min, reaction time is 6h ~ 10h, add terminator then, add inorganic nanometer powder again, low whipping speed is under 500r/min～1000r/min, and the reaction time is 0.5h ~ 3h, promptly makes the block polymer that contains polyolefin alcohol segment and polyolefinic acid sodium segment of hybrid inorganic material;
(2) step (1) gained block polymer is carried out wet spinning as spinning solution, through supersolidification, stretching, thermal finalization, acetalation, washing and drying process, fiber carries out sennit the most at last successively, promptly gets required product; Wherein:
Coagulation bath temperature is 30 ~ 50 ℃, and the sodium sulphate content that adds in the coagulating bath is 30 ~ 42wt%, and the time is 10 ~ 60s;
The stretch bath temperature is 90 ~ 99 ℃, and the aqueous sodium persulfate solution concentration that adds in the stretch bath is 365 ~ 370g/L, and draw ratio is 10 ~ 12 times;
Heat setting temperature is 200 ~ 245 ℃, and the processing time is 0.5 ~ 2min;
The acetalation agent that acetalation is used in handling is one to multiple kind in formaldehyde, acetaldehyde, propionic aldehyde or the butyraldehyde, and the concentration of acetalation agent is 25 ~ 35 g/L, and the sulfuric acid of 225 ~ 315g/L is catalyst, and 70 ~ 200 g/L sodium sulphate are made into the aqueous solution for the resistance sweller.
Beneficial effect of the present invention is: there is the carboxylated hydrophilic group on this functional material surface, is easy to the absorption of microorganism and ammonium ion, and microorganism depend on thereon after also difficult drop-off, thereby improved the denitrogenation and the biochemical of biomembrance process waste water treatment process.Because of it has added the part inorganic nano material, increasing surperficial roughness simultaneously, nano particle has slowed down the STRESS VARIATION when filler is subjected to water impact in the inner slight void that forms of filler, thereby also increased the fracture strength of this material, the effective storage life of this filler is increased, reduced cost of investment.Because there is the carboxylic acid sodium group in this material, can be considered cationic ion-exchange resin, with the ammonium radical ion generation ion-exchange in the waste water, thus the content of nitrogen in the more effective removal water.
The specific embodiment
Further explain technical scheme and the technique effect of inventing below in conjunction with example, but the enforcement of these examples and unrestricted other embodiment of the present invention, the present invention has a lot of different embodiments, has more than to be limited to content described in this specification.
Embodiment 1:
Sodium sulfocyanate 55%
Polyvinyl alcohol 17%
Sodium polymethacrylate 13%
Azodiisobutyronitrile 0.15%
Dodecyl sodium sulfate 1.7%
Tetrasodium salt of EDTA 0.15%
Imvite 13%
According to the above ratio sodium sulfocyanate, polyvinyl alcohol, sodium polymethacrylate, dodecyl sodium sulfate are joined in the reactor.The control reaction temperature is in the time of 60～70 ℃, add tetrasodium salt of EDTA termination polymerisation after adding azobisisobutyronitrile initiated polymerization 6h ~ 8h, add the nano imvite powder, polymerization time is about 0.5～2h again, and it is standby as spinning solution to obtain thick liquid.
The manufacturing procedure that this wet spinning carried out comprises: solidify, operation such as stretching, thermal finalization, acetalation, washing, drying.Coagulation bath temperature is 30 ~ 50 ℃, and sodium sulphate content is 30 ~ 42%, and the time is 10 ~ 60 s.The stretch bath temperature is got 90 ~ 99 ℃, and the aqueous sodium persulfate solution concentration of stretch bath is 365 ~ 370g/L.The aqueous sodium persulfate solution concentration of damp and hot stretch bath is 36.5%～37.5%, and the maximum tension multiple is 10 ~ 12 times.Heat setting temperature is 200 ~ 245 ℃, and the processing time is 0.5 ~ 2min.The acetalation agent that acetalation is handled is that formaldehyde, acetaldehyde, propionic aldehyde or butyraldehyde concentration are 25 ~ 35 g/L, and the sulfuric acid of 225 ~ 315g/L is catalyst, and 70 ~ 200 g/L sodium sulphate are made into the certain density aqueous solution for the resistance sweller.Fiber by carrying out sennit after washing, the drying, is woven into the filler of different shape again.
Embodiment 2
Sodium sulfocyanate 57%
POLYPROPYLENE GLYCOL 15%
Sodium polymethacrylate 10%
Azobisisobutyronitrile 0.2%
Neopelex 1.6%
Acetic acid 0.2%
Kaolin 16%
According to the above ratio with sulphur hydracid sodium, POLYPROPYLENE GLYCOL, sodium polymethacrylate, neopelex, join in the reactor.The control reaction temperature adds acetic acid behind the adding azobisisobutyronitrile initiated polymerization 7h and stops polymerisation in the time of 70～80 ℃, adds the nano kaoline powder, and polymerization time is about 1.5h again, and it is standby as spinning solution to obtain the water white transparency thick liquid.
The manufacturing procedure that this wet spinning carried out comprises: solidify, operation such as stretching, thermal finalization, acetalation, washing, drying.Coagulation bath temperature is 30 ~ 50 ℃, and sodium sulphate content is 30 ~ 42%, and the time is 10 ~ 60 s.The stretch bath temperature is got 90 ~ 99 ℃, and the aqueous sodium persulfate solution concentration of stretch bath is 365 ~ 370g/L.The aqueous sodium persulfate solution concentration of damp and hot stretch bath is 36.5%～37.5%, and the maximum tension multiple is 10 ~ 12 times.Heat setting temperature is 200 ~ 245 ℃, and the processing time is 0.5 ~ 2min.The acetalation agent that acetalation is handled is that formaldehyde, acetaldehyde, propionic aldehyde or butyraldehyde concentration are 25 ~ 35 g/L, and the sulfuric acid of 225 ~ 315g/L is catalyst, and 70 ~ 200 g/L sodium sulphate are made into the certain density aqueous solution for the resistance sweller.Fiber is woven into the filler of different shape by washing, carry out sennit after the drying.
Embodiment 3
Sodium sulfocyanate 50%
POLYPROPYLENE GLYCOL 21%
Sodium Polyacrylate 19%
Potassium peroxydisulfate 0.1%
Lauryl sodium sulfate 1.75%
Acetic acid 0.15%
Diatomite 18%
According to the above ratio with sulphur hydracid sodium, POLYPROPYLENE GLYCOL, Sodium Polyacrylate, lauryl sodium sulfate, join in the reactor.The control reaction temperature adds acetic acid behind the adding potassium peroxydisulfate initiated polymerization 8h and stops polymerisation in the time of 70～80 ℃, adds the nano diatomite powder, and polymerization time is about 1h again, and it is standby as spinning solution to obtain the water white transparency thick liquid.
The manufacturing procedure that this wet spinning carried out comprises: solidify, operation such as stretching, thermal finalization, acetalation, washing, drying.Coagulation bath temperature is 30 ~ 50 ℃, and sodium sulphate content is 30 ~ 42%, and the time is 10 ~ 60 s.The stretch bath temperature is got 90 ~ 99 ℃, and the aqueous sodium persulfate solution concentration of stretch bath is 365 ~ 370g/L.The aqueous sodium persulfate solution concentration of damp and hot stretch bath is 36.5%～37.5%, and the maximum tension multiple is 10 ~ 12 times.Heat setting temperature is 200 ~ 245 ℃, and the processing time is 0.5 ~ 2min.The acetalation agent that acetalation is handled is that formaldehyde, acetaldehyde, propionic aldehyde or butyraldehyde concentration are 25 ~ 35 g/L, and the sulfuric acid of 225 ~ 315g/L is catalyst, and 70 ~ 200 g/L sodium sulphate are made into the certain density aqueous solution for the resistance sweller.Fiber is woven into the filler of different shape by washing, carry out sennit after the drying.
Efficient denitrification filler among the present invention is obtained following effect:
(1) in the Processing Test of waste water, domestic ordinary elasticity filler needed 20 ~ 30 days carry out microorganism growth biofilm process, and on this microorganism compatibility denitrogenation filler 7 ~ 10 day time can finish. Contain the RCOONa group in this denitrogenation filler, has the ion exchange with NH4+, the NH4+ ion is adsorbed onto on the efficient denitrification filler, be convenient to nitrococcus, nitrifier is oxidized to NO2-N and NO3-N to NH3-N, promoted biological coordination to remove the effect of NH4+-N, reduce the concentration of NH4+-N in the waste water, improved the clearance of NH4+-N in the waste water. Added the inorganic nanometer-powder body in the functional material, the stress that nano particle has slowed down when filler is subjected to the current impact in the inner small space that forms of filler changes, thereby has increased the fracture strength of this material, increases the service life. The blend nano-powder can increase the roughness of fiber, makes the easier fiber surface that is adsorbed on of microorganism, and difficult drop-off has increased the compatibility of filler to microorganism.
(2) filler made of this functional material is mainly used in the biomembrance process wastewater treatment, is mainly used in the removal of nitrogen in the waste water. During use, filler 10 * 10cm rule is hung arrangement, cultivate acclimation sludge and also carry out biofilm, can form at filling surface after the filler biofilm and have certain thickness biomembrane, can form successively aerobic, anoxic, anaerobic environment, be equivalent to n little A2/O technology, more be conducive to the microorganism denitrogenation. Handled water flows through from the filler hole, contact filling surface microorganism, thus microorganism consumes the nitrogen element in the water, even water is purified.
(3) for the water body of surface water and slight pollution, the fixing row of branch of filler can be hung on and carry out denitrogenation in the water body and process and also can reduce CODMn simultaneously; And for wastewater from chemical industry such as Urethane Elastic Fibre Producing Waste Water, it can be deposited in the reactor. After the microorganism inoculation, can be adsorbed on rapidly filling surface, and spread growth, the microorganism after the maturation becomes can be with the whole biomembrane that coats of filler. This cultivation process approximately needs 7 ~ 10 days. After the biomembrane growth and maturity, has good removal ability by the decomposition of microorganism with to the pollutant such as organic matter, ammonia nitrogen in the water.
(4) this filler is positioned in the waste water, its to sanitary sewage CODCr clearance greater than 90%, the BOD5 clearance greater than 95%, the NH3-N(ammonia nitrogen) clearance is greater than 95%; The TN(total nitrogen) excursion of clearance is 86% ~ 95%, i.e. the denitrogenation effect of this efficient denitrification organic filler reaches GB18918-2002 one-level A discharge standard. After using this filler that microorganism is cultivated domestication in industrial wastewater, also can process industrial wastewater, such as the waste water of spandex factory. CODCr, BOD5 are the important overall target of evaluation water pollution degree, the chemical oxygen consumption (COC) that CODCr adopts potassium bichromate to determine as oxidant. BOD5 is BOD on the five, refers to the be degraded amount of oxygen of post consumption of organic matter that the microorganism in the water can degrade.
To sum up, functional material admixture of the present invention the inorganic nanometer-powder body, it is strong to have increased material surface roughness and hydrophily, microorganism is easy in its surface attachment growth, shorten microorganism and cultivate the domestication time, again because the surface have carboxylic acid sodium group can with waste water in the ammonium radical ion carry out ion-exchange, more effectively remove nitrogen pollutant in the water.
Claims (8)
1. ion-exchange type denitrification functions material is characterized in that described functional material is made up of solvent, polyolefin alcohol, polyolefinic acid sodium, initator, terminator, dispersant and inorganic nanometer powder, by weight percentage:
Solvent 25%～58%,
Polyolefin alcohol 10%～21%,
Polyolefinic acid sodium 10%～21%,
Initator 0.01%～0.8%,
Terminator 0.01%～0.2%,
Dispersant 2%～6%,
All the other are inorganic nanometer powder, and its gross weight satisfies 100%;
Ion-exchange type denitrification functions material according to claim 1 is characterized in that described solvent is a sodium sulfocynanate solution.
2. ion-exchange type denitrification functions material according to claim 1 is characterized in that described initator is azodiisobutyronitrile or potassium peroxydisulfate.
3. ion-exchange type denitrification functions material according to claim 1 is characterized in that described reactant polyolefin alcohol is in polyvinyl alcohol or the POLYPROPYLENE GLYCOL one to two kind.
4. ion-exchange type denitrification functions material according to claim 1 is characterized in that described reactant polyolefinic acid sodium is in Sodium Polyacrylate or the sodium polymethacrylate one to two kind.
5. ion-exchange type denitrification functions material according to claim 1 is characterized in that described terminator is acetic acid or tetrasodium salt of EDTA.
6. ion-exchange type denitrification functions material according to claim 1 is characterized in that described dispersant is one to several in lauryl sodium sulfate, neopelex, the dodecyl sodium sulfate.
7. ion-exchange type denitrification functions material according to claim 1 is characterized in that described inorganic nanometer powder is one to several in diatomite, kaolin or the imvite.
8. ion-exchange type denitrification functions preparation methods as claimed in claim 1 is characterized in that concrete steps are:
(1) with dissolution with solvents polyolefin alcohol, polyolefinic acid sodium, initator and dispersant, 60 ℃-85 ℃ and mixing speed is to carry out polymerisation under 200r/min～600r/min, reaction time is 6h-10h, add terminator then, add inorganic nanometer powder again, low whipping speed is under 500r/min～1000r/min, and the reaction time is 0.5h-3h, promptly makes the block polymer that contains polyolefin alcohol segment and polyolefinic acid sodium segment of hybrid inorganic material;
(2) step (1) gained block polymer is carried out wet spinning as spinning solution, through supersolidification, stretching, thermal finalization, acetalation, washing and drying process, fiber carries out sennit the most at last successively, promptly gets required product; Wherein:
Coagulation bath temperature is 30-50 ℃, and the sodium sulphate content that adds in the coagulating bath is 30-42wt%, and the time is 10-60s;
The stretch bath temperature is 90-99 ℃, and the aqueous sodium persulfate solution concentration that adds in the stretch bath is 365-370g/L, and draw ratio is 10-12 times;
Heat setting temperature is 200-245 ℃, and the processing time is 0.5-2min;
The acetalation agent that acetalation is used in handling is one to multiple kind in formaldehyde, acetaldehyde, propionic aldehyde or the butyraldehyde, and the concentration of acetalation agent is 25-35 g/L, and the sulfuric acid of 225-315g/L is catalyst, and 70-200 g/L sodium sulphate is made into the aqueous solution for the resistance sweller.
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Cited By (5)
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| CN102153205A (en) * | 2010-12-10 | 2011-08-17 | 江苏苏净集团有限公司 | Functional material for wastewater denitrification filler and preparation method thereof |
| CN105858749A (en) * | 2016-05-31 | 2016-08-17 | 陈萍 | Wastewater treating agent special for livestock breeding and preparing method of wastewater treating agent |
| CN107456956A (en) * | 2017-07-26 | 2017-12-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Polyester macromolecule/clay composite adsorbing material preparation method and products thereof and application |
| CN109748378A (en) * | 2017-11-06 | 2019-05-14 | 重庆干城环保科技有限公司 | A kind of production technology of making Nano surface bio-carrier |
| CN109748398A (en) * | 2017-11-06 | 2019-05-14 | 重庆干城环保科技有限公司 | A kind of production technology and bio-carrier of the bio-carrier that making Nano surface quantum biological can be implanted into |
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| CN101475251A (en) * | 2008-10-24 | 2009-07-08 | 江苏工业学院 | Composite denitrification agent for treating medium concentration ammonia nitrogen wastewater and denitrification method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153205A (en) * | 2010-12-10 | 2011-08-17 | 江苏苏净集团有限公司 | Functional material for wastewater denitrification filler and preparation method thereof |
| CN105858749A (en) * | 2016-05-31 | 2016-08-17 | 陈萍 | Wastewater treating agent special for livestock breeding and preparing method of wastewater treating agent |
| CN107456956A (en) * | 2017-07-26 | 2017-12-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Polyester macromolecule/clay composite adsorbing material preparation method and products thereof and application |
| CN107456956B (en) * | 2017-07-26 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of polyester polymer/clay composite adsorption material, product and application thereof |
| CN109748378A (en) * | 2017-11-06 | 2019-05-14 | 重庆干城环保科技有限公司 | A kind of production technology of making Nano surface bio-carrier |
| CN109748398A (en) * | 2017-11-06 | 2019-05-14 | 重庆干城环保科技有限公司 | A kind of production technology and bio-carrier of the bio-carrier that making Nano surface quantum biological can be implanted into |
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