CN106241998A - A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent - Google Patents
A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent Download PDFInfo
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- CN106241998A CN106241998A CN201610850195.8A CN201610850195A CN106241998A CN 106241998 A CN106241998 A CN 106241998A CN 201610850195 A CN201610850195 A CN 201610850195A CN 106241998 A CN106241998 A CN 106241998A
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- chinese medicine
- medicine dreg
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- reverse osmosis
- flocculation agent
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
Abstract
A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent, belongs to the technical field preparing natural composite flocculation agent.The present invention, with Chinese medicine dreg as raw material, obtains product through productions such as gas explosion process, extraction separation, cationization, washing are dried.The inventive method has that production technology is simple, stable, comprehensive resource utilization rate is high, raw material is easy to get and the feature such as cheap, unharmful substance discharge.The composite flocculation agent prepared of the inventive method is used to have stable performance, the feature such as safely and effectively.The product using the inventive method to produce, can be widely applied in the water treatment fields such as chemical industry.
Description
Technical field
The invention belongs to prepare the technical field of natural composite flocculation agent, prepare natural particularly to one Chinese medicine dreg
The method of composite flocculation agent.
Background technology
In water technology, flocculent precipitation is that one is widely used and requisite technology, and flocculant
It it is the key of flocculation sediment treatment effect quality.Natural organic high-molecular flocculant, owing to its raw material sources are extensive, price is low
Honest and clean, nontoxic, easily biological-degradable, form the advantages such as benign cycle at nature, be listed in environmentally friendly water treatment agent.Chinese medicines
Containing much starch, cellulose and protein in slag, medicinal residues amount utilizes greatly and the most effectively and develops, and causes a large amount of
The wasting of resources, used if can integrate, be not only and turn waste into wealth, also save process medicinal residues expense.
The existing method preparing natural composite flocculation agent, the notification number such as 06 month Granted publication on the 02nd in 2010 is CN
The patent of invention of 101284693B " natural organic polymer composite flocculant and production method thereof and application ", disclosed in this patent
Method is: first purple Cortex Cannabis or Chinese bandoline wood skin are pulverized, and then delivers into aquation compound reaction tank, adds clear water heating,
Disperse under stirring condition, add the chitosan solution after dissolving with rare organic acid, abundant compound reaction, more ground filter
Product.The major defect that the method exists has: 1. using heating aquation in production process, heating-up temperature is high, and heated time is long, holds
Easily coking, is not easy to produce continuously；2. chitosan is only blended by this technique with purple Cortex Cannabis or Chinese bandoline wood skin, does not enters polysaccharide
Row is structurally-modified so that it is flocculation ability is by a definite limitation；The most raw materials used chitosan is relatively costly, is used for by this flocculant
Cost of water treatment is the biggest；4. producing the composite flocculation agent obtained is colloidal, not readily transportable, stores the time short.
Summary of the invention
It is an object of the invention to the weak point for existing production composite flocculation agent method, it is provided that one Chinese medicine dreg
The method preparing natural composite flocculation agent, the method has that production technology is simple, stable, comprehensive resource utilization rate is high, raw material is easy
And the feature such as cheap, unharmful substance discharge.The composite flocculation agent using the inventive method to prepare has stable performance, peace
The feature such as the most effective.
The mechanism of the present invention is: steam explosion is to be placed in the environment of high temperature, high pressure by raw material, and raw material is by superheated liquid
Swollen, is full of steam in hole, when moment releases high pressure, the superheated liquid rapid vaporization in raw material hole, volume is the most swollen
Swollen and make cell " explosion ".Through this method pretreatment Chinese medicine dreg, the crystalline texture of raw material is broken, and the accessibility making reaction is notable
Increase, thus improve subsequent reactions efficiency.Cationic reagent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride not only can be with fiber
Hydroxyl generation nucleophilic displacement of fluorine in element, starch, also can be with-the NH in protein molecule2, the functional group such as-COOH ,-OH carry out sun
Ion reaction, so that cellulose, starch, protein cationization simultaneously, obtains composite flocculation agent.Meanwhile, ionizing is anti-
Ying Zhong, uses microwave-assisted, and molecule polarizes under electromagnetic field effect, and changes with the change of electromagnetic field, produces the higher-order of oscillation,
So relative motion between warm-up movement and the molecule of polar molecule itself can produce the similar work rubbing, colliding, vibrate, extrude
With, make place maximum system energy increase and be rapidly heated, so that reaction completes at short notice, and reduce in course of reaction
Organic solvent uses.Owing to needing waste water major part granule to be processed and colloid all with negative charge, cationic flocculant can
To play charging neutrality and adsorption bridging effect with microgranule in water, make de-steady, the flocculation of microgranule, contribute to sedimentation and filtering means dehydration.
The object of the present invention is achieved like this: a kind of Chinese medicine dreg prepares the method for natural composite flocculation agent, with in
Medicine medicinal residues are raw material, obtain product through productions such as gas explosion process, extraction separation, cationization, washing are dried.Its concrete side
Method step is as follows:
(1) gas explosion processes
With Chinese medicine dreg as raw material, first rustless steel autoclave is connected with high pressure steam generator, forms homemade steam
Demolition set.Then according still further to the quality (g) of Chinese medicine dreg: volume (mL) ratio of rustless steel autoclave is for 1:10's～30
Ratio, adds Chinese medicine dreg in rustless steel autoclave, then passes to high steam, until in still pressure reach 3.0～
Till during 6.0 MPa, press butterfly valve in opening after keeping 30～60 min, carry out gas explosion process, collect gas explosion Chinese medicine dreg.For
The gas explosion Chinese medicine dreg collected, processes for next step.Wherein, Chinese medicine dreg is pseudo-ginseng slag, Radix Astragali slag, Radix Codonopsis slag, and does not limits
In the Chinese medicine dreg enumerated.
(2) extraction separates
After (1st) step completes, according to the quality (g) of the gas explosion Chinese medicine dreg that (1st) step is collected: volume (mL) ratio of distilled water is
The ratio of 1:15～30, is scattered in gas explosion Chinese medicine dreg in distilled water, and low whipping speed is 150～200 r/min, and temperature is
Under conditions of 30～45 DEG C, extract 2～3 h.After extraction completes, extraction mixture is pumped in pressure filter, 0.20～0.30
Under MPa, controlling filter sizes is 200～400 mesh, carries out filter pressing.After filter pressing terminates, collect filtered solution and filtering residue respectively.For
The filtering residue collected, processes for next step；For the filtered solution collected, pump in reverse osmosis concentration device, 0.15～0.25
Under MPa, carry out reverse osmosis concentration, until the volume of reverse osmosis trapped fluid reduces to the 20～30% of original volume, collect respectively
Reverse osmosis permeate and reverse osmosis trapped fluid.Reverse osmosis permeate for collecting is distilled water, can be re-used for (2nd) step
Extraction；For the reverse osmosis trapped fluid collected, rich in water soluble protein, aminoacid, polysaccharide, trace element etc., chilled dry
Dry can be as animal feed additive.
(3) cationization
After (2nd) step completes, first according to 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: mass fraction be 20～30% NaOH water-soluble
Liquid volume ratio is the ratio of 1:10～15, and mix homogeneously obtains mixed liquor.Quality (g) according still further to the filtering residue that (2nd) step is collected: mixed
Close the ratio that volume (mL) ratio of liquid is 1:6～12, mixed liquor is sprayed onto rapidly on filtering residue, fully mixes.Then place into
In microwave reactor, under conditions of microwave power is 150～200 W, react 5～10 min, after having reacted, collect reaction
Product, processes for next step.
(4) washing is dried
After (3rd) step completes, the product that (3rd) step is collected, with absolute ethanol washing to neutral, collect cleaning mixture respectively
And washed-residue.Cleaning mixture for collecting can be re-used for washing after reclaiming ethanol；For the washed-residue collected, 40～50
It is dried at DEG C, obtains natural composite flocculation agent product.
After the present invention uses technique scheme, mainly have the following effects:
1, the natural composite flocculation agent that the present invention prepares, using natural medicinal residues is raw material, relative to traditional single flocculant
Flocculating effect more preferably, and is easily degraded, will not be to environment, safely and effectively.
2, the present invention is in process of production, uses steam blasting device and microwave reactor synergy, reaction can and
Property dramatically increases, and the product flocculating effect finally prepared is more preferable.
3, the present invention is in process of production, and with discarded Chinese medicine dreg as raw material, with low cost and refuse is turned waste into wealth；Produce
During material recycle recycle, and obtain feed additive side-product.
4, the present invention is in process of production, main uses self-control demolition set, microwave, the equipment such as is dried, produces equipment letter
Single, easy and simple to handle and easily controllable, therefore production safety reduces again production cost.
Detailed description of the invention
Below in conjunction with detailed description of the invention, further illustrate the present invention.
Embodiment 1
A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent, and concrete grammar step is as follows:
(1) gas explosion processes
With Chinese medicine dreg as raw material, first rustless steel autoclave is connected with high pressure steam generator, forms homemade steam
Demolition set.Then according still further to the quality (g) of Chinese medicine dreg: the volume (mL) of rustless steel autoclave is than the ratio for 1:10
Example, adds Chinese medicine dreg in rustless steel autoclave, then passes to high steam, until pressure reaches 3.0 MPa in still
Time till, press butterfly valve in opening after keeping 30 min, carry out gas explosion process, collect gas explosion Chinese medicine dreg.For the gas explosion collected
Chinese medicine dreg, processes for next step.Wherein, Chinese medicine dreg is pseudo-ginseng slag.
(2) extraction separates
After (1st) step completes, according to the quality (g) of the gas explosion Chinese medicine dreg that (1st) step is collected: volume (mL) ratio of distilled water is
The ratio of 1:15, is scattered in gas explosion Chinese medicine dreg in distilled water, and low whipping speed is 150 r/min, and temperature is the bar of 30 DEG C
Under part, extract 2 h.After extraction completes, pumping in pressure filter by extraction mixture, under 0.20 MPa, controlling filter sizes is
200 mesh, carry out filter pressing.After filter pressing terminates, collect filtered solution and filtering residue respectively.For the filtering residue collected, process for next step；
For the filtered solution collected, pump in reverse osmosis concentration device, under 0.15 MPa, carry out reverse osmosis concentration, until reverse osmosis cuts
The volume staying liquid reduces to the 20% of original volume, collects reverse osmosis permeate and reverse osmosis trapped fluid respectively.For collect
Reverse osmosis permeate is distilled water, can be re-used for the extraction of (2nd) step；For the reverse osmosis trapped fluid collected, rich in water-soluble
Property protein, aminoacid, polysaccharide, trace element etc., freeze-dried can be as animal feed additive.
(3) cationization
After (2nd) step completes, first according to 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: mass fraction is the NaOH aqueous liquid of 20%
The long-pending ratio ratio for 1:10, mix homogeneously obtains mixed liquor.Quality (g) according still further to the filtering residue that (2nd) step is collected: the body of mixed liquor
Long-pending (mL) ratio ratio for 1:6, is sprayed onto mixed liquor rapidly on filtering residue, fully mixes.Then place in microwave reactor,
Under conditions of microwave power is 150 W, react 5 min, after having reacted, collecting reaction product, process for next step.
(4) washing is dried
After (3rd) step completes, the product that (3rd) step is collected, with absolute ethanol washing to neutral, collect cleaning mixture respectively
And washed-residue.Cleaning mixture for collecting can be re-used for washing after reclaiming ethanol；For the washed-residue collected, at 40 DEG C
It is dried, obtains natural composite flocculation agent product.
Embodiment 2
A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent, and concrete grammar step is as follows:
(1) gas explosion processes
With Chinese medicine dreg as raw material, first rustless steel autoclave is connected with high pressure steam generator, forms homemade steam
Demolition set.Then according still further to the quality (g) of Chinese medicine dreg: the volume (mL) of rustless steel autoclave is than the ratio for 1:20
Example, adds Chinese medicine dreg in rustless steel autoclave, then passes to high steam, until pressure reaches 4.5 MPa in still
Time till, press butterfly valve in opening after keeping 45 min, carry out gas explosion process, collect gas explosion Chinese medicine dreg.For the gas explosion collected
Chinese medicine dreg, processes for next step.Wherein, Chinese medicine dreg is Radix Astragali slag.
(2) extraction separates
After (1st) step completes, according to the quality (g) of the gas explosion Chinese medicine dreg that (1st) step is collected: volume (mL) ratio of distilled water is
The ratio of 1:25, is scattered in gas explosion Chinese medicine dreg in distilled water, and low whipping speed is 180 r/min, and temperature is the bar of 40 DEG C
Under part, extract 2.5 h.After extraction completes, extraction mixture is pumped in pressure filter, under 0.25 MPa, control filter sizes
It is 300 mesh, carries out filter pressing.After filter pressing terminates, collect filtered solution and filtering residue respectively.For the filtering residue collected, at next step
Reason；For the filtered solution collected, pump in reverse osmosis concentration device, under 0.20 MPa, carry out reverse osmosis concentration, until reverse osmosis
The volume of trapped fluid reduces to the 25% of original volume, collects reverse osmosis permeate and reverse osmosis trapped fluid respectively.For collecting
Reverse osmosis permeate be distilled water, the extraction of (2nd) step can be re-used for；For the reverse osmosis trapped fluid collected, rich in water
Soluble proteins, aminoacid, polysaccharide, trace element etc., freeze-dried can be as animal feed additive.
(3) cationization
After (2nd) step completes, first according to 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: mass fraction is the NaOH aqueous liquid of 25%
The long-pending ratio ratio for 1:12, mix homogeneously obtains mixed liquor.Quality (g) according still further to the filtering residue that (2nd) step is collected: the body of mixed liquor
Long-pending (mL) ratio ratio for 1:9, is sprayed onto mixed liquor rapidly on filtering residue, fully mixes.Then place in microwave reactor,
Under conditions of microwave power is 180 W, react 8 min, after having reacted, collecting reaction product, process for next step.
(4) washing is dried
After (3rd) step completes, the product that (3rd) step is collected, with absolute ethanol washing to neutral, collect cleaning mixture respectively
And washed-residue.Cleaning mixture for collecting can be re-used for washing after reclaiming ethanol；For the washed-residue collected, at 45 DEG C
It is dried, obtains natural composite flocculation agent product.
Embodiment 3
A kind of Chinese medicine dreg prepares the method for natural composite flocculation agent, and concrete grammar step is as follows:
(1) gas explosion processes
With Chinese medicine dreg as raw material, first rustless steel autoclave is connected with high pressure steam generator, forms homemade steam
Demolition set.Then according still further to the quality (g) of Chinese medicine dreg: the volume (mL) of rustless steel autoclave is than the ratio for 1:30
Example, adds Chinese medicine dreg in rustless steel autoclave, then passes to high steam, until pressure reaches 6.0 MPa in still
Time till, press butterfly valve in opening after keeping 60 min, carry out gas explosion process, collect gas explosion Chinese medicine dreg.For the gas explosion collected
Chinese medicine dreg, processes for next step.Wherein, Chinese medicine dreg is Radix Codonopsis slag.
(2) extraction separates
After (1st) step completes, according to the quality (g) of the gas explosion Chinese medicine dreg that (1st) step is collected: volume (mL) ratio of distilled water is
The ratio of 1:30, is scattered in gas explosion Chinese medicine dreg in distilled water, and low whipping speed is 200 r/min, and temperature is the bar of 45 DEG C
Under part, extract 3 h.After extraction completes, pumping in pressure filter by extraction mixture, under 0.30 MPa, controlling filter sizes is
400 mesh, carry out filter pressing.After filter pressing terminates, collect filtered solution and filtering residue respectively.For the filtering residue collected, process for next step；
For the filtered solution collected, pump in reverse osmosis concentration device, under 0.25 MPa, carry out reverse osmosis concentration, until reverse osmosis cuts
The volume staying liquid reduces to the 30% of original volume, collects reverse osmosis permeate and reverse osmosis trapped fluid respectively.For collect
Reverse osmosis permeate is distilled water, can be re-used for the extraction of (2nd) step；For the reverse osmosis trapped fluid collected, rich in water-soluble
Property protein, aminoacid, polysaccharide, trace element etc., freeze-dried can be as animal feed additive.
(3) cationization
After (2nd) step completes, first according to 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: mass fraction is the NaOH aqueous liquid of 30%
The long-pending ratio ratio for 1:15, mix homogeneously obtains mixed liquor.Quality (g) according still further to the filtering residue that (2nd) step is collected: the body of mixed liquor
Long-pending (mL) ratio ratio for 1:12, is sprayed onto mixed liquor rapidly on filtering residue, fully mixes.Then microwave reactor is placed into
In, under conditions of microwave power is 200 W, react 10 min, after having reacted, collecting reaction product, at next step
Reason.
(4) washing is dried
After (3rd) step completes, the product that (3rd) step is collected, with absolute ethanol washing to neutral, collect cleaning mixture respectively
And washed-residue.Cleaning mixture for collecting can be re-used for washing after reclaiming ethanol；For the washed-residue collected, at 50 DEG C
It is dried, obtains natural composite flocculation agent product.
Hereinafter only do experiment with above-described embodiment 1, verify that the present invention produces by Kaolin waste water dam example
The effect of product.
It is configured to suspension that concentration is 500 mg/L to simulate sewage with commercially available Kaolin, first measures its primary cloudy
Degree；Then adding 5.0 mg composite flocculation agents in 1.0 L simulate sewage, controlling mixing speed is 200 r/min, quickly stirs
30 s, make flocculant dispersed；Reduce mixing speed the most again to 40 r/min, stop stirring after 30 min, staticly settle
30 min, take supernatant and survey its residual turbidity.Test result indicate that, composite flocculation agent to simulation sewage turbidity removal rate up to
81.7%。
It is last it should be noted that above example is only in order to illustrate technical scheme rather than restriction technologies side
Case, although the present invention has been described in detail by applicant with reference to preferred embodiment, those of ordinary skill in the art should
Understanding, technical scheme is modified or equivalent by those, without deviating from objective and the model of the technical program
Enclose, all should contain in the middle of scope of the presently claimed invention.
Claims (1)
1. the method preparing natural composite flocculation agent with Chinese medicine dreg, it is characterised in that concrete grammar step is as follows:
(1) gas explosion processes
With Chinese medicine dreg as raw material, first rustless steel autoclave is connected with high pressure steam generator, forms homemade steam
Demolition set；Then according still further to the quality of Chinese medicine dreg: the volume ratio of rustless steel autoclave is 1 g:10～the ratio of 30 mL
Example, adds Chinese medicine dreg in rustless steel autoclave, then passes to high steam, until pressure reaches 3.0～6.0 in still
Till during MPa, press butterfly valve in opening after keeping 30～60 min, carry out gas explosion process, collect gas explosion Chinese medicine dreg；Wherein, in
Medicine medicinal residues are pseudo-ginseng slag, Radix Astragali slag, Radix Codonopsis slag, and are not limited to the Chinese medicine dreg enumerated；
(2) extraction separates
After (1st) step completes, according to the quality of the gas explosion Chinese medicine dreg that (1st) step is collected: the volume ratio of distilled water is 1 g:15
～30 ratios of mL, gas explosion Chinese medicine dreg is scattered in distilled water, low whipping speed is 150～200 r/min, and temperature is
Under conditions of 30～45 DEG C, extract 2～3 h；After extraction completes, extraction mixture is pumped in pressure filter, 0.20～0.30
Under MPa, controlling filter sizes is 200～400 mesh, carries out filter pressing；After filter pressing terminates, collect filtered solution and filtering residue respectively；For
The filtered solution collected, pumps in reverse osmosis concentration device, under 0.15～0.25 MPa, carries out reverse osmosis concentration, until reverse osmosis
The volume of trapped fluid reduces to the 20～30% of original volume, collects reverse osmosis permeate and reverse osmosis trapped fluid respectively；
(3) cationization
After (2nd) step completes, first according to 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride: mass fraction be 20～30% NaOH water-soluble
Liquid volume ratio is the ratio of 1:10～15, and mix homogeneously obtains mixed liquor；Quality according still further to the filtering residue that (2nd) step is collected: mixing
The volume ratio of liquid is 1 g:6～the ratio of 12 mL, is sprayed onto rapidly on filtering residue by mixed liquor, fully mixes；Then place into micro-
In ripple reactor, under conditions of microwave power is 150～200 W, react 5～10 min, after having reacted, collect reaction and produce
Thing；
(4) washing is dried
After (3rd) step completes, the product that (3rd) step is collected, with absolute ethanol washing to neutral, collect cleaning mixture respectively
And washed-residue；For the washed-residue collected, it is dried at 40～50 DEG C, obtains natural composite flocculation agent product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610850195.8A CN106241998B (en) | 2016-09-26 | 2016-09-26 | A method of natural composite flocculation agent is prepared with Chinese medicine dreg |
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| CN201610850195.8A CN106241998B (en) | 2016-09-26 | 2016-09-26 | A method of natural composite flocculation agent is prepared with Chinese medicine dreg |
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| CN106241998A true CN106241998A (en) | 2016-12-21 |
| CN106241998B CN106241998B (en) | 2019-02-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106904713A (en) * | 2017-05-05 | 2017-06-30 | 遵义医学院 | A kind of water purification agent and preparation method thereof |
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|---|---|---|---|---|
| CN101514042A (en) * | 2009-03-23 | 2009-08-26 | 宋艳 | Method for preparing humic acid fish and veterinary drug preparations by traditional Chinese medicine residues |
| CN103610826A (en) * | 2013-12-05 | 2014-03-05 | 尚圣杰 | Hair-blacking kelp medicament and preparation method thereof |
| CN105692842A (en) * | 2016-04-13 | 2016-06-22 | 山西大学 | Application and preparation of flocculating agent for water bloom control |
| CN105800839A (en) * | 2014-12-29 | 2016-07-27 | 赵景歧 | Biogas residue liquid solid-liquid separation process |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514042A (en) * | 2009-03-23 | 2009-08-26 | 宋艳 | Method for preparing humic acid fish and veterinary drug preparations by traditional Chinese medicine residues |
| CN103610826A (en) * | 2013-12-05 | 2014-03-05 | 尚圣杰 | Hair-blacking kelp medicament and preparation method thereof |
| CN105800839A (en) * | 2014-12-29 | 2016-07-27 | 赵景歧 | Biogas residue liquid solid-liquid separation process |
| CN105692842A (en) * | 2016-04-13 | 2016-06-22 | 山西大学 | Application and preparation of flocculating agent for water bloom control |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106904713A (en) * | 2017-05-05 | 2017-06-30 | 遵义医学院 | A kind of water purification agent and preparation method thereof |
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Effective date of registration: 20210616 Address after: 570105 unit 403, block a, Hainan Binhai International Financial Center, 117 Binhai Avenue, Longhua District, Haikou City, Hainan Province Patentee after: Hainan Zhongxiang Technology Co.,Ltd. Address before: 400067 No. 19, Xuefu Avenue, Nan'an District, Chongqing Patentee before: CHONGQING TECHNOLOGY AND BUSINESS University |