CN102603081A - Preparation method of degradable cellulose base filler used for water treatment - Google Patents
Preparation method of degradable cellulose base filler used for water treatment Download PDFInfo
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- CN102603081A CN102603081A CN2012100899371A CN201210089937A CN102603081A CN 102603081 A CN102603081 A CN 102603081A CN 2012100899371 A CN2012100899371 A CN 2012100899371A CN 201210089937 A CN201210089937 A CN 201210089937A CN 102603081 A CN102603081 A CN 102603081A
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Abstract
The invention relates to water treatment filler in environmental protection field, in particular to a preparation method of degradable cellulose base filler used for water treatment. The preparation method is mainly as follows: fibers are prepared by technology of N-methyl morpholine-N-oxide, the mechanical property of the filler is improved further by the cross-linking and modifying technology, simultaneously, the surface of the filler is processed to load positive charge on the surface of the filler, so that the microorganism can adhere and grow on the surface of the filler conveniently. According to the invention, the method is simple and environment-friendly, the fibers prepared by the technology of N-methyl morpholine-N-oxide is good in mechanical property, and the prepared filler is large in superficial area, high in porosity, beneficial to protecting the growth of microorganisms, good in effect during the water treatment, and high in application value, and can not cause secondary pollution.
Description
Technical field
The present invention relates to the water treatment filler in environmental protection field, be specifically related to the preparation method of a kind of water treatment with the cellulose based degradable filler.
Background technology
Make waste water contact be grown in the lip-deep microbial film of stationary support, utilize biological degradation or transform that organic pollutant is a kind of method of wastewater treatment, i.e. a biomembrance process now commonly used in the waste water.Biologic packing material is the core in the microbial film water technology as the rely medium of growth and breeding of mikrobe.Filler that uses at present such as granulated active carbon, zeolite, silica sand, plastics, silica gel, Ceramic Balls etc.; The remaining residue in discarded back often contains a large amount of poisonous, objectionable impurities; Or be difficult to decompose, form solid waste, be prone to form secondary pollution, difficult treatment.
Utilizing Biodegradable material to handle waste water as biofilm carrier is a new technology; At patent CN 1765770A; Disclose the cellulose base bio-carrier of a kind of water treatment with controlled degradation, it belongs to the water treatment filler technical field, and the preparation of carrier is that Mierocrystalline cellulose is obtained the Mierocrystalline cellulose viscose glue through alkalization, sulfonation; Add whipping agent again, regeneration obtains the cellulose-based carrier filler in dilute acid soln; The controlled degradation modifying process of carrier is that this carrier and linking agent ethylene glycol diglycidylether is crosslinked, reaches the controllable modified purpose of degradation speed, with after do not produce environmental pollution.But in the carrier production process, by product H
2S, CS
2Make the fiber production complex proceduresization Deng emitting of obnoxious flavour, and polluted environment.Although the fiber of producing has the operation of one washing before drying, still can residual a part of sulfocompound in the fiber.Emitting also of obnoxious flavour can cause some other problem aborning, makes like the bubble in the fiber that intensity is inhomogeneous, the gathering of gas makes gelatinous fiber size that unpredictable variation take place, thereby product performance are descended.
Summary of the invention
The objective of the invention is to solve existing water treatment filler and produce secondary pollution problem, provide that a kind of preparation technology is simple, environmental protection, can make the preparation method of the water treatment of the good degradable filler product of performance simultaneously with the cellulose based degradable filler with the back.
In order to solve the problems of the technologies described above, the present invention is able to solve through following technical proposals:
Water treatment comprises the steps: with the preparation method of cellulose based degradable filler
Step a: cellulose materials is crushed to the 500-1000 order, and every gram Mierocrystalline cellulose powder adds 2-5ml water cut 30-50% N-methyl beautiful jade-N-oxide compound, mixes;
Step b: in N-methyl beautiful jade-N-oxide dissolution homogeneous fibre cellulosic material; In with the Mierocrystalline cellulose quality than (5-20): 10 ratio adds linking agent; Stir and leave standstill 40-60min, place 40-70 ℃ of water-bath heater to heat 50-240min in above mixture again;
Step c: controlled temperature is 35-40 ℃; In the filamentary material after crosslinked; Add again starch 2-5% in the Mierocrystalline cellulose quality, Mierocrystalline cellulose quality meter mikrobe 10-15%, account for the nutritive substance of microbial quality 5-10%, foaming, the cellulose wadding of moulding is dry down at 45-65 ℃;
Steps d: with the exsiccant cellulose wadding, be immersed in by the dried carrier of every gram in the mixing solutions of polymine and NaOH of 15-30ml, and be heated to 40-60 ℃, stirred 1 hour, take out with zero(ppm) water and clean, 45-65 ℃ of drying, product.
As preferably, the massfraction of the polymine in the described steps d is 40-50%; The massfraction of NaOH solution is 10%.
As preferably, described linking agent is a N-methylol amide amine linking agent.
As preferably, described linking agent is a N hydroxymethyl acrylamide.
As preferably, described mikrobe is amphimicrobe or anerobes.
As preferably, described nutritive substance be glucose, microcosmic salt, ammonium salt any.
As preferably, described cellulose materials is straw or wheat straw stalk.
The present invention has significant technique effect owing to adopted above technical scheme:
(1) product material Mierocrystalline cellulose of the present invention with low cost, be easy to get, production technique belongs to process for cleanly preparing, environmental friendliness;
(2) N-methyl beautiful jade-N-oxide compound has the dissolution conditions gentleness, and is high to the cellulose dissolution degree;
(3) carrier performance is good, has improved support strength through cross-linking modified technology, and handles through the surface to filler, makes it positively charged, more helps mikrobe in its surface adhesion, growth;
(4) filling surface is long-pending greatly, porosity is high, helps protecting microbial growth, and is effective during water treatment, and can not cause secondary pollution.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail:
Embodiment 1
1, straw is crushed to 800 orders, every gram straw powder adds 3ml water cut 35%N-methyl beautiful jade-N-oxide compound (NMMOH2O), mixes;
2, in the uniform rice-straw fibre cellulosic material of N-methyl beautiful jade-N-oxide dissolution, add the 0.5gN-NMA by every gram straw powder, stir and leave standstill 50min, place 60 ℃ of water-bath heaters to heat 120min in above mixture again;
3, controlled temperature is being 35 ℃; In the rice-straw fibre cellulosic material after crosslinked; Add 2% starch in the straw cellulose quality, 10% amphimicrobe of straw cellulose quality meter and the glucose of amphimicrobe massfraction 5% again; Foaming, the straw cellulose filler of moulding is dry down at 55 ℃.
4, exsiccant straw cellulose filler is immersed in the mixing solutions that 15ml concentration is 40% polymine and 10% (massfraction) NaOH by the dried carrier of every gram, 50 ℃ were stirred 1 hour down.Taking-up is cleaned with zero(ppm) water, 55 ℃ of dryings.
The straw cellulose packing specific area that obtains is 2380 m2/m3, and porosity is 87%, cellulose crosslinked degree 8.62%.
Embodiment 2
1, straw is crushed to 800 orders, every gram straw powder adds 3ml water cut 35%N-methyl beautiful jade-N-oxide compound (NMMOH2O), mixes;
2, in the uniform straw powder of N-methyl beautiful jade-N-oxide dissolution, add the 1.5gN-NMA by every gram straw cellulose, stir and leave standstill 50min, place 50 ℃ of water-bath heaters to heat 120min in above mixture again;
3, controlled temperature is being 35 ℃; In the rice-straw fibre cellulosic material after crosslinked, add again, account for the microcosmic salt of anerobes quality 8% in 3% starch of straw cellulose quality 12% anerobes as caking agent, straw cellulose quality meter; Foaming, the straw filler of moulding is dry down at 55 ℃.
4, exsiccant straw cellulose filler is immersed in 10% (massfraction) NaOH solution that 15ml concentration is 45% polymine by the dried carrier of every gram, 50 ℃ were stirred 1 hour down.Taking-up is cleaned with zero(ppm) water, 55 ℃ of dryings.
The straw cellulose packing specific area that obtains is 2754 m2/m3, and porosity is 91%, cellulose crosslinked degree 10.96%.
Embodiment 3
1, the wheat straw stalk is crushed to 800 orders, every gram wheat straw stalk powder adds 3ml water cut 35%N-methyl beautiful jade-N-oxide compound (NMMOH2O), mixes;
2, in the uniform wheat straw stalk of N-methyl beautiful jade-N-oxide dissolution, add the 2gN-NMA by every gram wheat straw stalk powder, stir and leave standstill 50min, place 50 ℃ of water-bath heaters to heat 120min in above mixture again;
3, controlled temperature is being 38 ℃; In the wheat straw stalk powder after crosslinked, add 4% starch in wheat straw fibre quality amount, 15% anerobes of wheat straw fibre quality amount meter again, account for the ammonium salt of anerobes quality 10%; Foaming, the plain filler of the wheat straw fibre of moulding is dry down at 55 ℃.
4, the plain filler of exsiccant wheat straw fibre is immersed in 10% (massfraction) NaOH solution that 15ml concentration is 50% polymine by the dried carrier of every gram, 60 ℃ were stirred 1 hour down.Taking-up is cleaned with zero(ppm) water, 55 ℃ of dryings.
The plain packing specific area of the wheat straw fibre that obtains is 2812 m2/m3, and porosity is 92%, cellulose crosslinked degree 11.34%.
In a word, the above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (7)
1. water treatment is characterized in that with the preparation method of cellulose based degradable filler, comprises the steps:
Step a: cellulose materials is crushed to the 500-1000 order, and every gram Mierocrystalline cellulose powder adds N-methyl beautiful jade-N-oxide compound of 2-5ml water cut 30-50%, mixes;
Step b: in N-methyl beautiful jade-N-oxide dissolution homogeneous fibre cellulosic material; In with the Mierocrystalline cellulose quality than (5-20): 10 ratio adds linking agent; Stir and leave standstill 40-60min, place 40-70 ℃ of water-bath heater to heat 50-240min in above mixture again;
Step c: controlled temperature is 35-40 ℃; In the filamentary material after crosslinked; Add again starch 2-5% in the Mierocrystalline cellulose quality, Mierocrystalline cellulose quality meter mikrobe 10-15%, account for the nutritive substance of microbial quality 5-10%, foaming, the cellulose wadding of moulding is dry down at 45-65 ℃;
Steps d: with the exsiccant cellulose wadding, be immersed in by the dried carrier of every gram in the mixing solutions of polymine and NaOH of 15-30ml, and be heated to 40-60 ℃, stirred 1 hour, take out with zero(ppm) water and clean, 45-65 ℃ of drying, product.
2. water treatment according to claim 1 is characterized in that with the preparation method of cellulose based degradable filler: the massfraction of the polymine in the described steps d is 40-50%; The massfraction of NaOH solution is 10%.
3. water treatment according to claim 1 is characterized in that with the preparation method of cellulose based degradable filler: described linking agent is a N-methylol amide amine linking agent.
According to claim 1 or 3 described water treatments with the preparation method of cellulose based degradable filler, it is characterized in that: described linking agent is a N hydroxymethyl acrylamide.
5. water treatment according to claim 1 is characterized in that with the preparation method of cellulose based degradable filler: described mikrobe is amphimicrobe or anerobes.
6. water treatment according to claim 1 is characterized in that with the preparation method of cellulose based degradable filler: described nutritive substance be glucose, microcosmic salt, ammonium salt any.
7. water treatment according to claim 1 is characterized in that with the preparation method of cellulose based degradable filler: described cellulose materials is straw or wheat straw stalk.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466782A (en) * | 2013-09-24 | 2013-12-25 | 四川环能德美科技股份有限公司 | High-affinity biological carrier |
| CN104542296A (en) * | 2015-01-16 | 2015-04-29 | 广东省农业科学院作物研究所 | Open rooting method for sugarcane tissue culture seedlings |
| CN105585730A (en) * | 2014-11-17 | 2016-05-18 | 成都安捷宜康环保科技有限公司 | Preparation method for novel cellulose carrier |
| CN111087068A (en) * | 2019-12-24 | 2020-05-01 | 南京公诚节能新材料研究院有限公司 | Preparation method of biological filter material for water purification treatment |
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| WO1999050193A1 (en) * | 1998-03-31 | 1999-10-07 | Samsung Engineering Co., Ltd. | Wastewater treatment method for removing organic matter and nitrogen, carrier used thereof and method for manufacturing the carrier |
| WO2003018166A1 (en) * | 2001-08-20 | 2003-03-06 | Zimmer Aktiengesellschaft | Method for removing heavy metals from media containing heavy metals by means of a lyocell moulded body, cellulosed moulded body comprising adsorbed heavy metals, and the use of the same |
| CN1562800A (en) * | 2004-04-22 | 2005-01-12 | 天津大学 | Stuffing of controllable degradative macropore cellulose for carrying microbe in use for treating wastewater and preparation |
| CN1723069A (en) * | 2002-10-10 | 2006-01-18 | 阿尔斯特罗姆研究及服务公司 | Filtering medium and use of the said filtering medium for pollution removal from lagoons |
| CN1765770A (en) * | 2005-09-06 | 2006-05-03 | 天津大学 | Degradation controllable cellulose base microbe carrier stuffing for water disposal and its preparation method |
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2012
- 2012-03-30 CN CN201210089937.1A patent/CN102603081B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999050193A1 (en) * | 1998-03-31 | 1999-10-07 | Samsung Engineering Co., Ltd. | Wastewater treatment method for removing organic matter and nitrogen, carrier used thereof and method for manufacturing the carrier |
| WO2003018166A1 (en) * | 2001-08-20 | 2003-03-06 | Zimmer Aktiengesellschaft | Method for removing heavy metals from media containing heavy metals by means of a lyocell moulded body, cellulosed moulded body comprising adsorbed heavy metals, and the use of the same |
| CN1723069A (en) * | 2002-10-10 | 2006-01-18 | 阿尔斯特罗姆研究及服务公司 | Filtering medium and use of the said filtering medium for pollution removal from lagoons |
| CN1562800A (en) * | 2004-04-22 | 2005-01-12 | 天津大学 | Stuffing of controllable degradative macropore cellulose for carrying microbe in use for treating wastewater and preparation |
| CN1765770A (en) * | 2005-09-06 | 2006-05-03 | 天津大学 | Degradation controllable cellulose base microbe carrier stuffing for water disposal and its preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466782A (en) * | 2013-09-24 | 2013-12-25 | 四川环能德美科技股份有限公司 | High-affinity biological carrier |
| CN103466782B (en) * | 2013-09-24 | 2016-08-10 | 四川环能德美科技股份有限公司 | A kind of high-affinity bio-carrier |
| CN105585730A (en) * | 2014-11-17 | 2016-05-18 | 成都安捷宜康环保科技有限公司 | Preparation method for novel cellulose carrier |
| CN104542296A (en) * | 2015-01-16 | 2015-04-29 | 广东省农业科学院作物研究所 | Open rooting method for sugarcane tissue culture seedlings |
| CN111087068A (en) * | 2019-12-24 | 2020-05-01 | 南京公诚节能新材料研究院有限公司 | Preparation method of biological filter material for water purification treatment |
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| CN102603081B (en) | 2014-03-05 |
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Address after: 310000 Xihu District, Hangzhou, Wen Wen Road No. 164, Hangzhou Institute of Commerce,, two Patentee after: ZHEJIANG SHUANGLIANG SHANGDA ENVIRONMENTAL PROTECTION Co.,Ltd. Address before: 310000 Xihu District, Hangzhou, Wen Wen Road No. 164, Hangzhou Institute of Commerce,, two Patentee before: ZHEJIANG SUNDA ENVIRONMENTAL PROTECTION Co.,Ltd. |
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Address after: Inside Hangzhou Business School, No.164 Wen'er Road, Xihu District, Hangzhou City, Zhejiang Province, 310000 Patentee after: Zhe JIANG Shuangliang Sunda Environment Protection Co.,Ltd. Address before: Inside Hangzhou Business School, No.164 Wen'er Road, Xihu District, Hangzhou City, Zhejiang Province, 310000 Patentee before: ZHEJIANG SHUANGLIANG SHANGDA ENVIRONMENTAL PROTECTION Co.,Ltd. |