CN107720843A - A kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant - Google Patents
A kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant Download PDFInfo
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- CN107720843A CN107720843A CN201711045413.1A CN201711045413A CN107720843A CN 107720843 A CN107720843 A CN 107720843A CN 201711045413 A CN201711045413 A CN 201711045413A CN 107720843 A CN107720843 A CN 107720843A
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- dosage
- dicyandiamide
- formaldehyde
- water
- decolorising agent
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The invention discloses a kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant, take formaldehyde and deionized water, it is added to and is equipped with the three-necked flask of agitator, thermometer, reflux condensing tube, start is stirring evenly and then adding into dicyandiamide and cyclohexylamine, stirs and is warming up to 50 DEG C, addition ammonium chloride, salt acid for adjusting pH value is used as 29 after reacting 20min, it is 40 DEG C 100 DEG C to be warming up to reaction temperature, is terminated after the 160min of question response time 80, cooling discharge.The present invention utilizes dicyandiamide and the initial reduced body of formaldehyde condensation polymer synthesizing water-solubility, a kind of dicyandiamide A formaldehyde cationic resins are formed by adding additive hexamethylene amine copolymer, and the influence factor such as dosage, temperature, pH to cyclohexylamine is analyzed, proved by a series of performance test, the waste water from dyestuff high-efficiency decolorant of preparation does not only reach low cost, dosage is small, and decolorizing efficiency is high, and final water quality is reached discharge standard.
Description
Technical field
The invention belongs to field, and in particular to a kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant.
Background technology
In the active dye wastewater of printing and dyeing mill, substantial amounts of anion is contained in dye molecule, is difficult to reality with general flocculant
The decolouring of existing waste water from dyestuff.Therefore, it is necessary to which the reactive dyed wastewater high-efficiency decolorant of exploitation has removing waste water from dyestuff face
The specific function of color.The present invention makes the negative electrical charge of institute's band on dye molecule be neutralized and unstability by providing substantial amounts of cation,
At the same time, the high-efficiency decolorant added generates substantial amounts of floccule because hydrolyzing, and it adsorbs, enlists the services of the dyestuff point after taking off surely
Son, and separated together from water body, so as to reach the purpose of decolouring.
The content of the invention
Goal of the invention：In order to solve the deficiencies in the prior art, the invention provides a kind of reactive dyed wastewater is efficient
The synthesis technique of decolorising agent.
Technical scheme：A kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant, it is described take 35% formaldehyde
16% and 60% deionized water, be added to equipped with agitator, thermometer, reflux condensing tube three-necked flask in, start stirring is equal
8% dicyandiamide and 2%-20% cyclohexylamine are added after even, stirs and is warming up to 50 DEG C, adds 2% ammonium chloride, reaction
With salt acid for adjusting pH value it is 2-9 after 20min, is warming up to reaction temperature as 40 DEG C -100 DEG C, is tied after question response time 80-160min
Beam, cooling discharge.
As optimization：The instrument of use is as follows：Electronic balance BSA-CW；Three-necked flask；DJIC gives power electric mixer；It is cold
Solidifying pipe, beaker, graduated cylinder, pipette；UV-1801 is ultraviolet/visible spectrophotometer；Sai Duolisi acidometers PB-10.
Beneficial effect：The present invention is using dicyandiamide and the initial reduced body of formaldehyde condensation polymer synthesizing water-solubility, by adding additive
Hexamethylene amine copolymer forms a kind of dicyandiamide-A- formaldehyde cationic resins, and the influence factor such as dosage, temperature, pH to cyclohexylamine
Analyzed, proved by a series of performance test, the waste water from dyestuff high-efficiency decolorant of preparation does not only reach low cost, dosage
Small, decolorizing efficiency is high, and final water quality is reached discharge standard.
Brief description of the drawings
Fig. 1 is influence schematic diagram of the ring amine dosage of the present invention to decolorizing effect；
Fig. 2 is influence schematic diagram of the reaction temperature of the present invention to decolorizing effect；
Fig. 3 is influence schematic diagram of the reaction time of the present invention to decolorizing effect.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, so that the technology of this area
Personnel can be better understood from advantages and features of the invention, so as to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only part of the embodiment of the present invention, rather than whole embodiments, based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained on the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
Embodiment
The present invention is using dicyandiamide and the initial reduced body of formaldehyde condensation polymer synthesizing water-solubility, by adding additive hexamethylene amine copolymer
A kind of dicyandiamide-A- formaldehyde cationic resins are formed, and the influence factor such as dosage, temperature, pH to cyclohexylamine is analyzed, and is led to
Crossing a series of performance test proves, the waste water from dyestuff high-efficiency decolorant of preparation does not only reach low cost, and dosage is small, decolorizing efficiency
Height, and final water quality is reached discharge standard.
The concrete technology of the present invention is as follows：
1. raw material：Dicyandiamide；35% formaldehyde；Cyclohexylamine, ammonium chloride, hydrochloric acid；Deionized water.
2. the instrument used is as follows：Electronic balance BSA-CW；Three-necked flask；DJIC gives power electric mixer；Condenser pipe, burning
Cup, graduated cylinder, pipette；UV-1801 is ultraviolet/visible spectrophotometer；Sai Duolisi acidometers PB-10.
3. synthesis technique：It is described take 35% the deionized water of formaldehyde 16% and 60%, be added to equipped with agitator, temperature
Count, in the three-necked flask of reflux condensing tube, start is stirring evenly and then adding into 8% dicyandiamide and 2%-20% cyclohexylamine, stirs
Mix and be warming up to 50 DEG C, add 2% ammonium chloride, it is 2-9 to react after 20min with salt acid for adjusting pH value, is warming up to reaction temperature
For 40 DEG C -100 DEG C, terminate after question response time 80-160min, cooling discharge.
4. each performance test and method are as follows：
4.1 solid content method of testings
Accurately weigh the constant flat measuring cup quality m of quality1；2~5g of sample, sample are accurately weighed with this measuring cup
M is designated as together with the quality of measuring cup2；Then the measuring cup equipped with sample is placed in baking oven and is dried to quality at 100~105 DEG C
Constant, now quality is designated as m3.Parallel test 3 times, takes the mean.Solid content X calculation formula：
4.2 decolorizing effect method of testings
1. titration：Experiment waste water 20ml is taken to adjust pH value to use buret to 8 to colorimetric cylinder (colourity 8000, COD 510)
Decolouring agent solution is added dropwise to Standard Colors, stands one minute, detection colourity (extension rate method) and COD, it is desirable to reach country one
Level discharge standard.
The medicament of preparation：Decolorising agent (2% solution, that is, diluting 50 times) to be measured
Decolorising agent dosage calculation formula：
Decolorising agent dosage (PPM)=【(decolorising agent dosage × diluted concentration/experiment wastewater volume】×106
★ PPM are hundred a ten thousandths, and dosage is that the added amount of chemical of the suitable 1 ton of waste water of 1PPM is 1 gram.
2. absorbance method：Using spectrophotometry, waste water is measured with ultraviolet-visible spectrophotometer continuous sweep method
Maximum absorption wavelength, at this wavelength measure decolourize before and after waste water absorbance, percent of decolourization calculating formula is percent of decolourization=(A0-
A)/A0× 100%
A0Absorbance before ----decolourize
Absorbance after A---- decolourings
After 4.3 decolourize, water-quality COD method of testing
Take active dye wastewaters of the 3.0ml after decolorising agent is handled to treat test sample, be placed in heating tubes of the 50ml with closed plug,
Screening agent is added, is mixed, 3.0ml digestion solutions and 5ml catalyst is then added, screws closed cover, is mixed.Heater connects electricity
Source, when being warming up to 165 DEG C, heating tube is put into heater, opens time switch, after 7 minutes, prepare liquid also reaches 165
DEG C when, heater can auto zero timing, automatically alarming after to be heated to 15 minutes.Heating tube is taken out, is added after cooling aobvious
Show agent, titrated with iron ammonium sulfate standard liquid.Do blank test simultaneously.COD cubage formula are as follows：
V0The iron ammonium sulfate consumption of ----blank
V1Iron ammonium sulfate consumption during ----water sample
V2The volume of ----water sample
The concentration of C---- iron ammonium sulfates
The molal weight of 8----1/2 oxygen
After 4.4 decolourize, water pH value method of testing
Respectively prepare 1% after decolorising agent is handled the active dye wastewater aqueous solution
(2) standard liquid acidity correction meter is used before test, blotted the surplus solution invested on electrode with filter paper, then use
Distilled water and prepare liquid washing electrode, then immerse electrode in test solution, and gently shake beaker, make solution uniform.Press
Read switch, start reading when numerical value change about in 10s is less than 0.01, the numerical value is the pH value of solution to be measured.Parallel examination
Test three times, average.Measurement finishes, and closes power supply, rinses electrode, glass electrode immersion.
5. result is with discussing
Influence of the 5.1 cyclohexylamine dosages to decolorizing effect
The addition of cyclohexylamine can reduce the synthesis cost of dicyandiamine-formaldehyde decolouriser, and cyclohexylamine is with formaldehyde in acid bar
Reaction generation high molecular polymer under part, the negative electrical charge that the polymer can be on neutralization activity dye molecule, there is net to catch bridge formation
Effect, the reactive dye that can be effectively combined in dyeing waste water, reaches decolouring purpose.
Fig. 1 is influence schematic diagram of the ring amine dosage of the present invention to decolorizing effect, is specially to certain printing and dyeing mill's colourity
8000 degree of active dye wastewater is tested, and when 35% formaldehyde dosage is 16%, the dosage of deionized water is 60%, double cyanogen
The dosage of amine is 8%, and the dosage of ammonium chloride is 2%, and temperature is 95 DEG C during synthesis, generated time 140min, when pH is 5, hexamethylene
Influence of the amine dosage to decolorizing effect：It will be seen from figure 1 that the dosage of cyclohexylamine, at 14%, decolorising agent dosage is minimum, effect
Preferably, that is, in 8000 degree of active dye wastewater, the dosage of decolorising agent is 125g/ tons.But when cyclohexylamine dosage is
When 18%, percent of decolourization is declined slightly, and this is probably gel occur because made decolorising agent molecular mass is excessive, causes it in water
In hydrolysis efficiency reduce, reduce decolorizing effect.
Influence of 5.2 reaction temperatures to bleaching agent bleaching effect
Reaction temperature mainly influences the stability of sintetics, and temperature is too low, and reaction is incomplete, and product stability is bad,
Easily produce precipitation or form jelly；Opposite thermal is too high, and C-N keys on dicyandiamide hydrolyze, while divides with multiple formaldehyde
Son reacts and crosslinked, and generation side chain, which makes strand be obstructed, to be stretched, so as to influence " to build bridge " effect decoloration performance
Reduce..
Fig. 2 is influence schematic diagram of the reaction temperature of the present invention to decolorizing effect, specially when 35% formaldehyde dosage is
16%, the dosage of water is 60%, and the dosage of dicyandiamide is 8%, and the dosage of cyclohexylamine is 14%, and the dosage of ammonium chloride is 2%, pH
For 5 when, generated time 140min, influence of the reaction temperature to product decolorizing effect during synthesis：Conclusion as can be drawn from Figure 2, when
Reaction temperature is controlled at 90 DEG C, and decolorising agent effect is best.
Influence of 5.3 pH value to decolorising agent stability
PH value is also very big to the stability influence of decolorising agent, and in the basic conditions, dicyandiamide-hexamethylene amine-for-aldehyde reaction is not
Completely, occur oligomeric or do not gather, not only stability is bad, and decolorizing effect is also bad.Conversely, under solutions of weak acidity, dicyandiamide first
Aldehyde reaction forms high molecular polymer, and reaction is complete, and effect and stability are good.
Table 1 is that the dosage of water is 60%, and the dosage of dicyandiamide is 8%, cyclohexylamine when 35% formaldehyde dosage is 16%
Dosage is 14%, and the dosage of ammonium chloride is 2%, when temperature is 95 DEG C during synthesis, influence of the pH value to decolouring stability during synthesis：
Influence of the pH value of table 1 to decolouring stability
As can be drawn from Table 4, as 4≤pH≤6 of decolorising agent, its own stability is good.
Influence of 5.4 reaction time to product decoloration performance
Synthesis of the reaction time to dicyandiamine-formaldehyde decolouriser has considerable influence, and the reaction time is too short, and condensation reaction is endless
Entirely, the viscosity of product is relatively low.And the flocculating effect of dicyandiamine-formaldehyde decolouriser has substantial connection with its viscosity, viscosity is bigger, shape
Into alumen ustum it is bigger, flocculating effect also better adjust respectively the reaction time for 80,100,120,140,160min be made products.
Influence schematic diagram from Fig. 3 reaction time to decolorizing effect can be seen that the reaction time in 120min, and decolorising agent dosage is bright
It is aobvious to reduce, good decolorizing effect, as the increase decolorising agent dosage in reaction time has been reduced but DeGrain.Therefore the reaction time
Control is preferred in 140min.
6. the performance test results contrast
6.1 decolorizing effects contrast
Table 2 is waste water of the colourity more than 8000 degree, uses same amount sample decolorising agent 1#、2#And the decolorising agent of research and development
Action effect contrasts：It will be tested for the ease of measure after 4 times of wastewater dilution.
The percent of decolourization contrast of the decolorising agent of table 2
It can be obtained from the data of upper table 2, for active dye wastewater decolorization, the decolorising agent of research and development is than sample decolorising agent 1#
With 2#Decolorizing effect it is more notable.
6.2 solid contents contrast
The sample decolorising agent 1 of table 3#With 2#With the solid content Comparative result of the decolorising agent of research and development：
The solid content Comparative result of the decolorising agent of table 3
Sample decolorising agent 1 is can be seen that from table 3#、2#Decolorising agent solid content than department's research and development is all much higher, but decolourizes
Effect is not as the decolorising agent of research and development.
After 6.3 decolourize, the contrast of water-quality COD test result
Table 4 is respectively through sample decolorising agent 1#With 2#After the decolorising agent processing of research and development, the contrast of water-quality COD test result：
The active dye wastewater COD contrasts after the processing of various decolorising agents respectively of table 4
| Before processing water-quality COD (mg/l) | Water-quality COD (mg/l) after processing | |
| Sample decolorising agent 1# | 510 | 72 |
| Sample decolorising agent 2# | 510 | 68 |
| Research and develop decolorising agent | 510 | 56 |
It can be drawn from table 4, after decolorising agent is handled, the COD contents in waste water can greatly reduce, from upper table data also
It can be seen that waste water decoloring agent more great Cheng of the reactive dyed wastewater high-efficiency decolorant researched and developed herein than Liang Zhong samples company
The COD reduced in waste water of degree, has reached country-level discharge standard.
After 6.4 decolourize, water pH value contrast
Table 5 is respectively through sample decolorising agent 1#With 2#After the decolorising agent processing researched and developed with company, water pH value test result pair
Than：
Active dye wastewater pH value contrast after 5 three kinds of decolorising agent processing of table
| Before processing water quality pH | Water quality pH after processing | |
| Sample decolorising agent 1# | 10.56 | 8.7 |
| Sample decolorising agent 2# | 10.56 | 7.9 |
| Research and develop decolorising agent | 10.56 | 7.5 |
It can draw from table 5, after decolorising agent is handled, a certain degree of pH value reduced in waste water of three, reach
National waste water first grade discharging requires (pH=6~9).
6.5 stability test Comparative results
Table 6 is sample decolorising agent 1#With 2#The stability for the decolorising agent researched and developed with company contrasts：
6 three kinds of decolorising agent stability contrasts of table
It can show that three kinds of decolorising agent self stabilities are good from table 6, three is acidproof intolerant to highly basic.
Reactive dyed wastewater high-efficiency decolorant of the present invention has stability good, and cost is low, and dosage is few, and effect is good
Advantage, it is specific as follows：
(1) it is de- to synthesizing by the dosage of the height of experimental study reaction temperature, the size of pH value, cyclohexylamine and each component
The influence of toner stability and decolorizing effect, preferably going out optimal synthesis technique is：95 DEG C, time 140min of temperature, 4≤pH≤6,
Formaldehyde dosage is 16%, water consumption 60%, and dicyandiamide dosage is 8%, and the dosage of cyclohexylamine is 14%, and ammonium chloride dosage is
2%.
(2) sample 1 more salable with the market is passed through#、2#Various performance comparisons are carried out, the decolorising agent of research and development has containing solid
Measure the characteristics of low, stability is good, good decolorizing effect；After decolorising agent is handled, the water-quality COD of three, pH value have reached state
Family's discharge of wastewater requirement.
Invention advantage：
1st, the present invention, which adds cyclohexylamine, can reduce the synthesis cost 20% of dicyandiamine-formaldehyde decolouriser.
2nd, the decolorising agent and the similar decolorising agent of market sale that the optimal synthesis technique that the present invention is drawn by testing synthesizes
Compared to the cost that can reduce by 15%.
3rd, the decolorising agent that the present invention synthesizes has extraordinary stability and resistance to acids and bases.
Claims (2)
- A kind of 1. synthesis technique of reactive dyed wastewater high-efficiency decolorant, it is characterised in that：It is described take 35% formaldehyde 16% and 60% deionized water, be added to equipped with agitator, thermometer, reflux condensing tube three-necked flask in, start stirring is equal 8% dicyandiamide and 2%-20% cyclohexylamine are added after even, stirs and is warming up to 50 DEG C, adds 2% ammonium chloride, reaction With salt acid for adjusting pH value it is 2-9 after 20min, is warming up to reaction temperature as 40 DEG C -100 DEG C, is tied after question response time 80-160min Beam, cooling discharge.
- 2. the synthesis technique of reactive dyed wastewater high-efficiency decolorant according to claim 1, it is characterised in that：Using Instrument it is as follows：Electronic balance BSA-CW；Three-necked flask；DJIC gives power electric mixer；Condenser pipe, beaker, graduated cylinder, liquid relief Pipe；UV-1801 is ultraviolet/visible spectrophotometer；Sai Duolisi acidometers PB-10.
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Cited By (1)
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