CN101215033A - Method for preparing ecological type composite flocculant by using straw - Google Patents

Method for preparing ecological type composite flocculant by using straw Download PDF

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Publication number
CN101215033A
CN101215033A CNA2008100520956A CN200810052095A CN101215033A CN 101215033 A CN101215033 A CN 101215033A CN A2008100520956 A CNA2008100520956 A CN A2008100520956A CN 200810052095 A CN200810052095 A CN 200810052095A CN 101215033 A CN101215033 A CN 101215033A
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China
Prior art keywords
stalk
sodium hydroxide
solution
straws
mass ratio
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CNA2008100520956A
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Chinese (zh)
Inventor
杨晓霞
周启星
华涛
王铁良
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南开大学
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Priority to CNA2008100520956A priority Critical patent/CN101215033A/en
Publication of CN101215033A publication Critical patent/CN101215033A/en

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Abstract

The invention relates to the field of sewage disposal and feed water purifying, specially is an ecotype highly active flocculating agent used for dealing trade waste or domestic sewage and purifying drinking water. The invention uses straws and nonorganic aluminum salt as basic raw materials, water as reaction solvent, and uses sodium hydroxide and chloroactic acid to modify straws, modified products makes complex response with aluminum salt to reduce ecological toxicity in nonorganic aluminum salt, and strengthens the flocculating performance of products, thereby causing the prepared novel products have the characteristics of ecological security, high efficiency and the like. The specific preparing method is, use sodium hydroxide solution to basify straws, then use chloroactic acid solution to etherify straws, use the income matter and nonorganic aluminum salt solution with specific proportion to be mixed and to proceed complex response, and adjust addition quantity of sodium hydroxide and chloroactic acid, mass ratio of straws and nonorganic aluminum salt, reaction temperature and time and the like according to reaction process, finally achieve a novel product. The invention uses straws as main raw materials, and has the advantages of low costs, cheapness, high efficiency, wide application, no secondary pollution, being environment-friendly and the like.

Description

A kind of method of utilizing stalk to prepare ecological type composite flocculant

Technical field

The present invention relates to sewage disposal and feedwater field, specifically a kind of environmental composite efficient flocculant that is used for trade effluent or sanitary sewage disposal and drink water purifying.

Background technology

Current, the flocculation agent of widespread use can be divided into kinds such as inorganic flocculating agent, organic floculant, microbial flocculant and composite flocculation agent in sewage disposal.Wherein inorganic flocculating agent is cheap, and flocculating effect is better, is representative with aluminium salt, molysite and polymkeric substance thereof; Alumen ustum density and intensity that molysite forms are bigger, purifying water effect is remarkable, be subjected to the water temperature impact effect little, pH value use range is wide, some former water is had treatment effect preferably, but the molysite flocculation agent not only has intensive corrodibility, to the equipment requirements height, and easy residual iron ion, make treating water have color, influence treatment effect; When processing contains the more trade effluent of sulfide, the Fe in the molysite flocculation agent 3+Be reduced into Fe 2+, and combine with sulphur and to generate FeS and Fe 2S 3Mixture, make flocculation activity forfeiture.In addition, contain a large amount of mineral ions in the water body that utilizes the mineral-type flocculation agent to handle, excessive mineral ion not only has influence on the mouthfeel of water quality, also is unfavorable for HUMAN HEALTH, thereby needs to increase desalination, deionization technology in the water supply process.The aluminum salt flocculant flocculating effect is also good, but aluminium wherein is after each channel enters human body, by accumulating and participating in many biochemical reactions, nutritive element essential in the body and trace element displacement can be run off or deposition, disturb and destroy the physiological function at each position, cause human body to occur such as clinical poisoning by aluminum illnesss such as aluminum encephalopathy, aluminium osteopathy, aluminium anaemias.Simultaneously, the toxicity of aluminium salt also shows the toxic effect to hydrobiont, plant.When the concentration of aluminium is big, also may produce detrimentally affect to the microorganism in the biological wastewater treatment process.The World Health Organization is 0.2mg/L to the limitation standard of residual aluminum content in the water, and the U.S. is decided to be 0.05mg/L, and also in provisional water quality standard in 2000, the standard value that has increased aluminium is 0.2mg/L in China.

Organic floculant comprises synthetic polymeric flocculant and natural macromolecule flocculating agent.The synthetic polymeric flocculant is representative with the polyacrylamide, and they are popular on market because flocculating effect is good, adding less.But the flocculation agent of these types has also brought very big pressure to environment in production, use and subsequent disposal, and human beings'health has been constituted obviously or potential harm.Available data shows: the synthetic organic polymer coargulator polyacrylamide that range of application is the widest, usage quantity is maximum at present is a low toxicity, though most commodity are skin irritation not, but some hydrolysis body has remaining alkalescence, repeatedly, have pungency when contacting for a long time.In addition, its synthetic cost high and also in building-up process acrylamide monomer and the toxic heavy metal carried secretly very big to human health damage, use the most of polymer in back to be difficult to by environment degradable, a large amount of accumulation and long-term existence are brought huge pressure to environment in physical environment; Small portion can be degraded to small molecules such as acrylamide monomer then is a toxic substance, has abundant to studies have shown that it is a kind ofly to poison the very strong material of nervosa, and has very strong carinogenicity, and human health is constituted a threat to.Common people's toxicological harmless daily ingested dose is 0.5mg/kg.The polyacrylamide maximum permitted concentration of U.S.'s approval is 1.0mg/L, when levels of residual monomers surpasses 0.5% (mass ratio), just should stick the label of " poisonous substance " in the packing of product of PAM.It is 0.5mg/L that Britain's regulation polyacrylamide on average adds concentration, and maximum dosage must not surpass 1mg/L, and acrylamide should be less than 0.05% at the residual volume of polymkeric substance.

Natural macromolecule flocculating agent mainly comprises natural organic high-molecular materials such as starch, tannin, polyose, chitosan class, xylogen, Mierocrystalline cellulose and gelatin, makes by chemical modification.Because the natural organic high-molecular material has nontoxic, energy safe disposal and lower-price characteristic once once causing the attention of each scientific research institution, but pure natural polyose parent material molecular weight are lower and unstable, consumption is big, and flocculating effect is not good and might produce problems such as BOD.Both at home and abroad the researchist attempts the natural polysaecharides material with organic molecule grafting such as acrylamides, and the mixture that obtains has stronger flocculating effect.But the secondary pollution of acrylamide monomer and biology toxicity problem still fail effectively to be solved, the preparation process complexity, and production cost also so greatly raises.Causing for many years can real business-like product and few in this field.

Microbial flocculant is that a class is by the special polymer meta-bolites that is difficult for the coagulation sedimentations such as solid suspended particle, somatic cells and colloidal particle of degraded in the made liquid of microorganisms.Utilize biotechnology, by microbial fermentation, extracting, refining obtaining.But the screening of existing microbial bacterial, cultivate, fermentation and extract the method for agglutinating matter and production process complexity, production cost too high, present stage mostly also is in laboratory stage, it is also unrealistic to implement extensive industrialization.

Because traditional inorganic polymer flocculant and synthetic organic polymer flocculation agent exists some inherent shortcomings, microbial flocculant is large-scale application not always also, composite flocculation agent has obtained development rapidly in recent years, especially it can overcome many deficiencies of using single flocculation agent, had the advantage of single flocculation agent concurrently, wide accommodation, to lower concentration or high-concentration waste water, colorful wastewater, various industrial sewage, sanitary wastewaters etc. all have good decontamination effect improving, can also improve organic clearance in the flocculation process, and can reduce the kish ionic concn, reduce secondary pollution.Therefore, composite flocculation agent has development prospect very widely.Natural organic high-molecular flocculant is because molecular weight is big, active group is many, structure is diversified and raw material sources are extensive, cheap, be easy to characteristics such as biological degradation, non-secondary pollution, in recent years, be used for developing novel flocculant by the lot of domestic and foreign research worker.Problems such as though inorganic flocculating agent has consumption big, and sedimentation time is slow, and is residual, cheap with become production art relatively advantage such as maturation also make it that very big application space was still arranged in today.Inorganic-natural polymer composite flocculation agent has both advantages especially concurrently, therefore also is the focus of composite flocculation agent development.

Summary of the invention

The object of the present invention is to provide a kind of economy, efficient, non-secondary pollution particularly reduces the ecologic type high efficient composite flocculation agent of the ecological risk that causes because of aluminium by the usage quantity that reduces aluminium preparation method.

To achieve these goals, the technical solution used in the present invention is: with stalk, inorganic aluminate is raw material, it particularly is major ingredient with the stalk, sodium hydroxide, Mono Chloro Acetic Acid are basifier and etherifying agent, and inorganic aluminate is made natural organic matter and inorganic aluminate composite flocculation agent as the parent base substance; According to the difference of the character of disposing of sewage, can in proper range, adjust formula for a product;

The preparation method is as follows:

A. process alkalizes

With crushed stalk, take by weighing the certain mass stalk powder in beaker, the sodium hydroxide solution of preparation 17~25%, slowly added this sodium hydroxide solution in the beaker in 1: 1~1: 100 by stalk and sodium hydroxide mass ratio, on magnetic stirring apparatus, stir, alkalized 50~60 minutes down in 20~40 ℃ of temperature condition;

B. etherification procedure

Compound concentration is 10~14% chloroacetic acid solution, presses stalk and Mono Chloro Acetic Acid mass ratio and added this chloroacetic acid solution in 1: 2~1: 100 in above-mentioned reaction solution, stirs, and temperature is adjusted into 70~80 ℃, carries out etherificate, and the time is 40~55 minutes;

C. complex reaction

The preparation inorganic aluminum salting liquid, solvent is Tai-Ace S 150, aluminum chloride or aluminum nitrate, concentration is 30~65%, mass ratio by stalk and inorganic aluminate in through the above-mentioned reaction solution of alkalization and etherificate is 1: 0.1~1: 10 adding inorganic aluminum salting liquid, temperature condition is controlled to be 40~90 ℃, reaction times is 1~9 hour, the beige liquid product, can concentrate as required or dry.

The present invention has the following advantages:

1. flocculating effect is good.Be in particular in: compare with commercially available inorganic aluminate processing trade effluent or sanitary sewage, flocculating effect of the present invention is equivalent to 1~2 times of common inorganic aluminate;

2. applied widely.Be applicable to various industrial sewage and sanitary wastewater, even the water supply industry water, and can further enlarge use range by adjusting formula rate;

3. ecological security.The present invention is the polymer composite flocculant that is made by rice straw and inorganic aluminate, product and inorganic aluminate after the stalk modification are compound, change aluminum ions combining form, the concentration of active aluminum is reduced greatly, the probability of small organic contamination deposits yields free radical reduces greatly in the aluminium salt ion catalysis water body, reduces to greatest extent even has eliminated aluminium salt toxicity;

4. non-secondary pollution.The employing stalk is a raw material, and the flocculation agent residue is easy to do not had the secondary pollution problem by the microbiological deterioration in the environment;

5. the preparation method is simple.This method is not high to equipment requirements, and the reaction conditions gentleness is easy to amplify, and realizes suitability for industrialized production;

6. economic performance is good, and cost is low.Stalk and inorganic aluminate are synthesis material of the present invention, and the source is wide, and price is low, " green " of stalk are used meet recycling economy, the needs of cleaner production.

Embodiment

The present invention is described in more detail below by embodiment.

Embodiment 1

The present invention is a raw material with stalk, inorganic aluminate (aluminum chloride) and water, and wherein stalk and aluminium salt are major ingredient, and water is as reaction solvent; Use sodium hydroxide and Mono Chloro Acetic Acid as basifier and etherifying agent stalk to be carried out modification, its preparation method is as follows:

(1) take by weighing stalk powder 1.5 grams, in the 250ml beaker, prepare 20% sodium hydroxide solution, slowly add this sodium hydroxide solution of 20ml in beaker, fully stir, alkalize under 40 ℃ of temperature condition, the time is 55 minutes;

(2) compound concentration is 13% chloroacetic acid solution, adds this chloroacetic acid solution 25ml in above-mentioned reaction solution, stirs, and carries out etherificate under 75 ℃ of conditions of temperature, and the time is 50 minutes;

(3) compound concentration is 60% aluminum trichloride solution, adds this aluminum trichloride solution of 25ml in through the above-mentioned reaction solution of alkalization and etherificate, stirs, temperature condition is controlled to be 40 ℃, carries out complex reaction, and the reaction times is 1 hour, get beige liquid product, i.e. product flocculation agent.

Embodiment 2

Difference from Example 1 is: stalk quality, addition amount of sodium hydroxide, Mono Chloro Acetic Acid add-on are different with complex reaction time.Its preparation method is as follows:

(1) take by weighing stalk powder 0.5 gram,, prepare 20% sodium hydroxide solution, slowly add this sodium hydroxide solution of 50ml in beaker, fully stir in the 250ml beaker,, under 40 ℃ of temperature condition, to alkalize, the time is 55 minutes;

(2) compound concentration is 13% chloroacetic acid solution, adds this chloroacetic acid solution 50ml in above-mentioned reaction solution, stirs, and carries out etherificate under 75 ℃ of temperature condition of temperature, and the time is 50 minutes;

(3) compound concentration is 60% aluminum trichloride solution, adds this aluminum trichloride solution of 25ml in through the above-mentioned reaction solution of alkalization and etherificate, stirs, temperature condition is controlled to be 40 ℃, carries out complex reaction, and the reaction times is 3 hours, get beige liquid product, i.e. product flocculation agent.

Embodiment 3

Difference from Example 2 is: stalk quality, addition amount of sodium hydroxide, Mono Chloro Acetic Acid add-on, complex reaction time are different with temperature.Its preparation method is as follows:

(1) take by weighing stalk powder 3 grams, in the 250ml beaker, prepare 20% sodium hydroxide solution, slowly add this sodium hydroxide solution of 40ml in beaker, fully stir, alkalize under 40 ℃ of temperature condition, the time is 55 minutes;

(2) compound concentration is 13% chloroacetic acid solution, adds this chloroacetic acid solution 35ml in above-mentioned reaction solution, stirs, and carries out etherificate under 75 ℃ of temperature condition of temperature, and the time is 50 minutes;

(3) compound concentration is 60% aluminum trichloride solution, adds this aluminum trichloride solution of 25ml in through the above-mentioned reaction solution of alkalization and etherificate, stirs, temperature condition is controlled to be 50 ℃, carries out complex reaction, and the reaction times is 7 hours, get beige liquid product, i.e. product flocculation agent.

Embodiment 4

Difference from Example 3 is: stalk quality, naoh concentration, Mono Chloro Acetic Acid concentration, complex reaction time are different with temperature.Its preparation method is as follows:

(1) take by weighing stalk powder 2 grams,, prepare 18% sodium hydroxide solution, slowly add this sodium hydroxide solution of 40ml in beaker, fully stir in the 250ml beaker,, under 40 ℃ of temperature condition, to alkalize, the time is 55 minutes;

(2) compound concentration is 14% chloroacetic acid solution, adds this chloroacetic acid solution 35ml in above-mentioned reaction solution, stirs, and carries out etherificate under 75 ℃ of temperature condition of temperature, and the time is 50 minutes;

(3) compound concentration is 60% aluminum trichloride solution, adds this aluminum trichloride solution of 25ml in through the above-mentioned reaction solution of alkalization and etherificate, stirs, temperature condition is controlled to be 80 ℃, carries out complex reaction, and the reaction times is 4 hours, get beige liquid product, i.e. product flocculation agent.

Claims (7)

1. ecologic type high efficient composite flocculation agent, it is characterized in that: with stalk powder and aluminium salt is raw material, and sodium hydroxide solution and chloroacetic acid solution are basifier and etherifying agent, and water is implemented preparation with method as follows as reaction solvent:
A) alkalization process: take by weighing the certain mass stalk powder, press the sodium hydroxide solution of stalk and sodium hydroxide mass ratio adding 17~25% in 1: 1~1: 150, stir, alkalized 40~70 minutes down in 20 ℃~40 ℃ temperature condition;
B) etherification procedure: pressed stalk and Mono Chloro Acetic Acid mass ratio 1: 2~1: 120, and in above-mentioned reaction solution, added 10~15% chloroacetic acid solution, in 70~80 ℃ of following etherificates of temperature condition 40~60 minutes;
C) recombination process: adding concentration by mass ratio 1: 0.1~1: 15 in through the above-mentioned reaction solution of alkalization and etherificate is 20~70% inorganic aluminum salting liquid, in the reaction 1~10 hour down of 30~90 ℃ of temperature condition, gets the beige liquid product.
2. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: described stalk is the common rice stalk, and its pulverizing is obtained stalk powder;
3. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: described inorganic aluminate can be Tai-Ace S 150, aluminum chloride or aluminum nitrate;
4. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: the concentration of the employed sodium hydroxide solution of alkalization process is 18~22%, and stalk and sodium hydroxide mass ratio 1: 1~1: 100, alkalization time are 50~65 minutes;
5. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: the concentration of the employed chloroacetic acid solution of etherification procedure is 10~14%, stalk and Mono Chloro Acetic Acid mass ratio 1: 2~1: 100, etherification temperature are 70~80 ℃, and the etherificate time is 40~55 minutes;
6. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: the mass ratio of described stalk and inorganic aluminate is 1: 0.1~1: 10;
7. according to the described environmental composite efficient flocculant of claim 1, it is characterized in that: in the recombination process, temperature is controlled to be 40 ℃~90 ℃, and the reaction times is 1~9 hour.
CNA2008100520956A 2008-01-17 2008-01-17 Method for preparing ecological type composite flocculant by using straw CN101215033A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102276037A (en) * 2011-08-12 2011-12-14 南开大学 Method for preparing environment-friendly and efficient composite flocculant
CN102295337A (en) * 2011-06-04 2011-12-28 江南大学 Printing and dyeing wastewater processing technology by quaternary ammonium salt cationic flocculant prepared by the use of straws
CN105731561A (en) * 2016-02-29 2016-07-06 济南大学 Light fiber water treatment conditioner prepared from palm kernel cakes
CN105731560A (en) * 2016-02-29 2016-07-06 济南大学 Composite light fiber water treatment conditioner prepared from wheat bran
CN105731621A (en) * 2016-02-29 2016-07-06 济南大学 Biomass coupling coagulant aid synthesized by fungus chaffs and plantasan
CN105753127A (en) * 2016-02-29 2016-07-13 济南大学 Biomass fiber coagulant aid prepared from beanstalk-semen cassiae gum
CN105753077A (en) * 2016-02-29 2016-07-13 济南大学 Biomass coupling water treatment conditioner prepared from bean pulp
CN106242006A (en) * 2016-10-17 2016-12-21 徐州工程学院 A kind of modified straw flocculant critical material and technical method thereof
CN106315805A (en) * 2016-10-17 2017-01-11 徐州工程学院 Modified straw polypropylene composite flocculant and key production technology thereof
CN106497572A (en) * 2016-10-10 2017-03-15 河西学院 A kind of solid water based on full corn straw and preparation method thereof
CN109048123A (en) * 2018-09-08 2018-12-21 佛山市禅城区诺高环保科技有限公司 A kind of preparation method for adulterating the chitosan-based scaling powder of magnalium silver element plant fiber

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102295337A (en) * 2011-06-04 2011-12-28 江南大学 Printing and dyeing wastewater processing technology by quaternary ammonium salt cationic flocculant prepared by the use of straws
CN102295337B (en) * 2011-06-04 2013-06-26 江南大学 Printing and dyeing wastewater processing technology by quaternary ammonium salt cationic flocculant prepared by the use of straws
CN102276037A (en) * 2011-08-12 2011-12-14 南开大学 Method for preparing environment-friendly and efficient composite flocculant
CN105731561A (en) * 2016-02-29 2016-07-06 济南大学 Light fiber water treatment conditioner prepared from palm kernel cakes
CN105731560A (en) * 2016-02-29 2016-07-06 济南大学 Composite light fiber water treatment conditioner prepared from wheat bran
CN105731621A (en) * 2016-02-29 2016-07-06 济南大学 Biomass coupling coagulant aid synthesized by fungus chaffs and plantasan
CN105753077A (en) * 2016-02-29 2016-07-13 济南大学 Biomass coupling water treatment conditioner prepared from bean pulp
CN105753127A (en) * 2016-02-29 2016-07-13 济南大学 Biomass fiber coagulant aid prepared from beanstalk-semen cassiae gum
CN106497572A (en) * 2016-10-10 2017-03-15 河西学院 A kind of solid water based on full corn straw and preparation method thereof
CN106497572B (en) * 2016-10-10 2019-10-22 河西学院 A kind of solid water and preparation method thereof based on full corn stover
CN106242006A (en) * 2016-10-17 2016-12-21 徐州工程学院 A kind of modified straw flocculant critical material and technical method thereof
CN106315805A (en) * 2016-10-17 2017-01-11 徐州工程学院 Modified straw polypropylene composite flocculant and key production technology thereof
CN109048123A (en) * 2018-09-08 2018-12-21 佛山市禅城区诺高环保科技有限公司 A kind of preparation method for adulterating the chitosan-based scaling powder of magnalium silver element plant fiber

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