CN105858849A - Method for removing Congo red flocculation decolorizing agent in printing and dyeing wastewater - Google Patents

Method for removing Congo red flocculation decolorizing agent in printing and dyeing wastewater Download PDF

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Publication number
CN105858849A
CN105858849A CN201610208968.2A CN201610208968A CN105858849A CN 105858849 A CN105858849 A CN 105858849A CN 201610208968 A CN201610208968 A CN 201610208968A CN 105858849 A CN105858849 A CN 105858849A
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mixed
stirring
reaction
powder
congo red
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裴俊
盛海丰
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Changzhou Dingri Environmental Protection Technology Co Ltd
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Changzhou Dingri Environmental Protection Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2618Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
    • C08G65/2621Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
    • C08G65/2624Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aliphatic amine groups
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Removal Of Specific Substances (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention discloses a method for removing a Congo red flocculation decolorizing agent in printing and dyeing wastewater, and belongs to the technical field of wastewater treatment. The method comprises the following steps: by taking nickel nitrate, aluminum nitrate, silver nitrate and magnesium nitrate as raw materials, mixing in an absolute ethyl alcohol solution containing urea, stirring to react in a reaction kettle, cooling, washing, calcining, and grinding so as to obtain hydrotalcite powder, adding diethanol amine and octadecy trimethyl ammonium bromide, stirring to react, dripping sodium hydroxide to generate precipitate, calcining and grinding, mixing with epoxy chloropropane, titrating by using dimethylamine, further adding an organic initiator, and performing polymerization reaction and curing, thereby obtaining the flocculation decolorizing agent. The method has the beneficial effects that the preparation steps are simple, a prepared product is high in removal efficiency on wastewater of which COD is less than 300mg/L, the removal rate is greater than 99.6%, and the product is good in pertinence; and no further deep oxidation treatment is needed, and the cost is 22% less than that of other methods.

Description

A kind of remove the preparation method of Congo red flocculating decoloring agent in dyeing waste water
Technical field
The present invention relates to a kind of remove the preparation method of Congo red flocculating decoloring agent in dyeing waste water, belong to technical field of waste water processing.
Background technology
Decolorization flocculation agent is a kind of to integrate decolouring, the novel quaternary amine type organic polymer coargulator of the COD etc. that flocculates, removes.Dicandiamide-formaldehyde cationic polymer decolorization flocculation agent is the additive reaction carrying out formaldehyde and dicyandiamide under certain condition, generates methylol dicyandiamide, carries out two polycondensation reactions of methylol compound the most under certain conditions.The DF polymer that synthetic reaction is generated contains amino, when they are put in waste water, not only can neutralize the negative charge of micelle in waste water, and micelle adsorption bridging can be reached the effect of flocculation, and the amino on polymer molecule can generate firm ion chain with the interphase interaction of the anionic group such as the sulfonic group in dye molecule, form water-fast macromolecular compound.On the negatron particle of the colloidal impurity that this compounds is attracted in water, form bulky grain, thus reach flocculating effect.
The preparation method of flocculating decoloring agent is to add dicyandiamide, carbamide and ammonium chloride in the three-neck flask equipped with reflux condensing tube and agitator at present, stirring, open condensed water, it is dividedly in some parts formalin, warming-in-water makes temperature in three-neck flask be 32e, reaction proceeds by, and period is with exothermic phenomenon.Stopping heating, the reaction heat that in dependence flask, reactant produces makes reaction temperature slowly rise.The release of question response heat adds remaining formalin after peak, is progressively warming up to predetermined reaction temperature, cools down, obtain water white transparency, liquid soluble in water, with stickiness, good fluidity is flocculating decoloring agent after reaction.The clearance that this flocculating decoloring agent is higher than 300 mg/L to waste water COD is higher, but when COD value drops to 300 mg/L, removes effect poor, clearance is low, further deep oxidation need to be made process and can be only achieved emission request, cause the process time long, the problem such as cost increase.
Summary of the invention
nullThe technical problem to be solved: clearance waste water COD being higher than 300 mg/L for dicandiamide-formaldehyde cationic polymer flocculating decoloring agent is higher,But when COD value drops to 300 mg/L,Removal effect is poor,Clearance is low,And need to make further deep oxidation process can be only achieved emission request,Cause the process time long,The drawback that cost increases,Provide a kind of with nickel nitrate、Aluminum nitrate、Silver nitrate and magnesium nitrate are raw material,Mixing is dissolved in urea-containing ethanol solution,In reaction kettle for reaction after stirring,Cooled、Washing、Calcining、Mill prepared brucite powder,Add diethanolamine、Cetyltrimethylammonium bromide stirring reaction,Dropping sodium hydroxide,Generate precipitate,Mill through calcining,Mix with epoxychloropropane,Titrate by dimethylamine,Add the aggregated reaction of organic initiators、Ripening prepares the method for flocculating decoloring agent.Preparation process of the present invention is simple, and products obtained therefrom is high less than 300 mg/L waste water removal efficiency to COD, reaches more than 99.6%, with strong points.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) 10~15g nickel nitrates, 12~13g aluminum nitrate, 8~10g silver nitrate and 8~12g magnesium nitrates are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the 100~180mL ethanol solutions containing 0.03~0.04mol carbamide, stirring 1~2h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 138~156 DEG C, reacts 14~16h;
(2) after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 3~5 times, putting into after washing and be dried 6~8h in 60~70 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 500~700 DEG C, calcining 2~3h, it is subsequently placed in mill and mills 1~2h, cross 80~100 mesh sieves, obtain brucite powder;
(3) in the brucite powder of above-mentioned gained, it is separately added into 30~40mL diethanolamine and 25~35mL Cetyltrimethylammonium bromides, stirring reaction 1~2h, dropping 10~12mL mass fractions are 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stand 1~2h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 600~700 DEG C, calcines 3~4h, calcined material being milled, sieve to obtain mixed-powder;
(4) in the mixed-powder of above-mentioned gained, add 100~120mL epoxychloropropane, stir 20~30min so that it is after being sufficiently mixed uniformly, controlling temperature is 3~7 DEG C, 8~10mL dimethylamine are dripped wherein with 2~3/s speed, after dropping, stirring reaction 1~2h;
(5) after reaction to be mixed, it is added thereto to mixed-powder quality 0.3~0.5% lauroyl peroxide in step (3), at 75~85 DEG C, polyreaction 2~3h, after polyreaction, being placed in temperature is at 100~125 DEG C, ripening 3~5h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.
The application process of the present invention: the Congo red flocculating decoloring agent in dyeing waste water of the removing present invention prepared adds to containing in the Congo red dyeing waste water that mass concentration is 50~290mg/L, addition is 3~5mg/L, stirring reaction 1~3h, dyeing waste water color gradually becomes water white transparency, in waste water after water outlet, Congo red mass concentration is reduced to 0.19~1.61mg/L, clearance reaches more than 99.6%, is worthy to be popularized and uses.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and products obtained therefrom is high less than 300 mg/L waste water removal efficiency to COD, reaches more than 99.6%, with strong points;
(2) processing without further deep oxidation, cost is less than additive method more than 22%.
Detailed description of the invention
First 10~15g nickel nitrates, 12~13g aluminum nitrate, 8~10g silver nitrate and 8~12g magnesium nitrates are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the 100~180mL ethanol solutions containing 0.03~0.04mol carbamide, stirring 1~2h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 138~156 DEG C, reacts 14~16h;Then after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 3~5 times, putting into after washing and be dried 6~8h in 60~70 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 500~700 DEG C, calcining 2~3h, it is subsequently placed in mill and mills 1~2h, cross 80~100 mesh sieves, obtain brucite powder;30~40mL diethanolamine and 25~35mL Cetyltrimethylammonium bromides it are separately added in the brucite powder of above-mentioned gained, stirring reaction 1~2h, dropping 10~12mL mass fractions are 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stand 1~2h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 600~700 DEG C, calcines 3~4h, calcined material being milled, sieve to obtain mixed-powder;In the mixed-powder of above-mentioned gained, add 100~120mL epoxychloropropane again, stir 20~30min so that it is after being sufficiently mixed uniformly, controlling temperature is 3~7 DEG C, 8~10mL dimethylamine are dripped wherein with 2~3/s speed, after dropping, stirring reaction 1~2h;After last reaction to be mixed, it is added thereto to mixed-powder quality 0.3~0.5% lauroyl peroxide, at 75~85 DEG C, polyreaction 2~3h, after polyreaction, being placed in temperature is at 100~125 DEG C, ripening 3~5h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.
Example 1
First 10g nickel nitrate, 12g aluminum nitrate, 8g silver nitrate and 8g magnesium nitrate are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the ethanol solution that 100mL contains 0.03mol carbamide, stirring 1h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 138 DEG C, reacts 14h;Then after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 3 times, putting into after washing and be dried 6h in 60 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 500 DEG C, calcining 2h, it is subsequently placed in mill the 1h that mills, crosses 80 mesh sieves, obtain brucite powder;30mL diethanolamine and 25mL Cetyltrimethylammonium bromide it is separately added in the brucite powder of above-mentioned gained, stirring reaction 1h, dropping 10mL mass fraction is 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stands 1h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 600 DEG C, calcines 3h, calcined material being milled, sieve to obtain mixed-powder;Adding 100mL epoxychloropropane again in the mixed-powder of above-mentioned gained, stir 20min so that it is after being sufficiently mixed uniformly, controlling temperature is 3 DEG C, drips 8mL dimethylamine wherein with 2/s speed, after dropping, and stirring reaction 1h;After last reaction to be mixed, being added thereto to mixed-powder quality 0.3% lauroyl peroxide, at 75 DEG C, polyreaction 2h, after polyreaction, being placed in temperature is at 100 DEG C, ripening 3h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.The Congo red flocculating decoloring agent in dyeing waste water of the removing present invention prepared adds to containing in the Congo red dyeing waste water that mass concentration is 50mg/L, addition is 3mg/L, stirring reaction 1h, dyeing waste water color gradually becomes water white transparency, in waste water after water outlet, Congo red mass concentration is reduced to 0.19mg/L, clearance reaches 99.62%, is worthy to be popularized and uses.
Example 2
First 13g nickel nitrate, 13g aluminum nitrate, 9g silver nitrate and 10g magnesium nitrate are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the ethanol solution that 140mL contains 0.04mol carbamide, stirring 2h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 147 DEG C, reacts 15h;Then after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 4 times, putting into after washing and be dried 7h in 65 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 600 DEG C, calcining 3h, it is subsequently placed in mill the 2h that mills, crosses 90 mesh sieves, obtain brucite powder;35mL diethanolamine and 30mL Cetyltrimethylammonium bromide it is separately added in the brucite powder of above-mentioned gained, stirring reaction 2h, dropping 11mL mass fraction is 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stands 2h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 650 DEG C, calcines 4h, calcined material being milled, sieve to obtain mixed-powder;Adding 110mL epoxychloropropane again in the mixed-powder of above-mentioned gained, stir 25min so that it is after being sufficiently mixed uniformly, controlling temperature is 5 DEG C, drips 9mL dimethylamine wherein with 3/s speed, after dropping, and stirring reaction 2h;After last reaction to be mixed, being added thereto to mixed-powder quality 0.4% lauroyl peroxide, at 80 DEG C, polyreaction 3h, after polyreaction, being placed in temperature is at 113 DEG C, ripening 4h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.The Congo red flocculating decoloring agent in dyeing waste water of the removing present invention prepared adds to containing in the Congo red dyeing waste water that mass concentration is 170mg/L, addition is 4mg/L, stirring reaction 2h, dyeing waste water color gradually becomes water white transparency, in waste water after water outlet, Congo red mass concentration is reduced to 0.51mg/L, clearance reaches 99.70%, is worthy to be popularized and uses.
Example 3
First 15g nickel nitrate, 13g aluminum nitrate, 10g silver nitrate and 12g magnesium nitrate are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the ethanol solution that 180mL contains 0.04mol carbamide, stirring 2h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 156 DEG C, reacts 16h;Then after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 5 times, putting into after washing and be dried 8h in 70 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 700 DEG C, calcining 3h, it is subsequently placed in mill the 2h that mills, crosses 100 mesh sieves, obtain brucite powder;40mL diethanolamine and 35mL Cetyltrimethylammonium bromide it is separately added in the brucite powder of above-mentioned gained, stirring reaction 2h, dropping 12mL mass fraction is 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stands 2h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 700 DEG C, calcines 4h, calcined material being milled, sieve to obtain mixed-powder;Adding 120mL epoxychloropropane again in the mixed-powder of above-mentioned gained, stir 30min so that it is after being sufficiently mixed uniformly, controlling temperature is 7 DEG C, drips 10mL dimethylamine wherein with 3/s speed, after dropping, and stirring reaction 2h;After last reaction to be mixed, being added thereto to mixed-powder quality 0.5% lauroyl peroxide, at 85 DEG C, polyreaction 3h, after polyreaction, being placed in temperature is at 125 DEG C, ripening 5h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.The Congo red flocculating decoloring agent in dyeing waste water of the removing present invention prepared adds to containing in the Congo red dyeing waste water that mass concentration is 290mg/L, addition is 5mg/L, stirring reaction 3h, dyeing waste water color gradually becomes water white transparency, in waste water after water outlet, Congo red mass concentration is reduced to 1.61mg/L, clearance reaches 99.79%, is worthy to be popularized and uses.

Claims (1)

1. remove the preparation method of Congo red flocculating decoloring agent in dyeing waste water for one kind, it is characterised in that concrete preparation process is:
(1) 10~15g nickel nitrates, 12~13g aluminum nitrate, 8~10g silver nitrate and 8~12g magnesium nitrates are weighed, it is uniformly mixed under 120r/min, collect mixture, mixture is dissolved in the 100~180mL ethanol solutions containing 0.03~0.04mol carbamide, stirring 1~2h, to be mixed complete after, stirring thing is poured in reactor, controlling temperature in reactor is 138~156 DEG C, reacts 14~16h;
(2) after question response completes, reactant is put in frozen water and be cooled to room temperature, and with ethanol and deionized water cyclic washing 3~5 times, putting into after washing and be dried 6~8h in 60~70 DEG C of vacuum drying ovens, put in Muffle furnace by dried object after drying, controlling temperature in Muffle furnace is 500~700 DEG C, calcining 2~3h, it is subsequently placed in mill and mills 1~2h, cross 80~100 mesh sieves, obtain brucite powder;
(3) in the brucite powder of above-mentioned gained, it is separately added into 30~40mL diethanolamine and 25~35mL Cetyltrimethylammonium bromides, stirring reaction 1~2h, dropping 10~12mL mass fractions are 30% sodium hydroxide solution the most wherein, after reaction to be mixed, stand 1~2h, precipitate is collected by filtration subsequently, and put the precipitate in Muffle furnace, controlling temperature in Muffle furnace is 600~700 DEG C, calcines 3~4h, calcined material being milled, sieve to obtain mixed-powder;
(4) in the mixed-powder of above-mentioned gained, add 100~120mL epoxychloropropane, stir 20~30min so that it is after being sufficiently mixed uniformly, controlling temperature is 3~7 DEG C, 8~10mL dimethylamine are dripped wherein with 2~3/s speed, after dropping, stirring reaction 1~2h;
(5) after reaction to be mixed, it is added thereto to mixed-powder quality 0.3~0.5% lauroyl peroxide in step (3), at 75~85 DEG C, polyreaction 2~3h, after polyreaction, being placed in temperature is at 100~125 DEG C, ripening 3~5h, i.e. prepares one and removes Congo red flocculating decoloring agent in dyeing waste water.
CN201610208968.2A 2016-04-06 2016-04-06 Method for removing Congo red flocculation decolorizing agent in printing and dyeing wastewater Withdrawn CN105858849A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112573550A (en) * 2020-11-24 2021-03-30 衢州学院 Method for preparing magnesium-based flame retardant by utilizing Grignard wastewater

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112573550A (en) * 2020-11-24 2021-03-30 衢州学院 Method for preparing magnesium-based flame retardant by utilizing Grignard wastewater

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