CN105858837A - Flocculating agent for chemical wastewater and preparation method thereof - Google Patents

Abstract

The invention discloses a flocculant for chemical wastewater and a preparation method thereof. The raw materials of the flocculant for chemical wastewater include: 20-30 parts of nonionic monomers, 3-5 parts of anionic monomers, and 3-5 parts of cationic monomers 10-20 parts, 2-4 parts of dimethylaminoethyl methacrylate monomer, 0.05-0.09 parts of initiator, 0.3-0.5 parts of ammonium persulfate, 120-140 parts of deionized water, 20-40 parts of fly ash ; The non-ionic monomer is acrylamide, methacrylamide and nitrogen substitutes thereof. The present invention has a higher density of charged groups, stronger adsorption and capture ability for colloids and suspended particles in water, high temperature resistance, high salt resistance, acid and alkali resistance, high broad spectrum and good stability compared with other flocculants. The flocculation effect is good. When used in sewage treatment, it has higher decolorization effect and higher DOD removal effect, and achieves the comprehensive treatment effect of sewage, which not only enhances the effect of chemical treatment of sewage, but also makes fly ash become waste. Treasures have been comprehensively utilized.

Description

A kind of flocculant for chemical wastewater and preparation method thereof

technical field

The invention relates to a chemical reagent, in particular to a flocculant for chemical waste water and a preparation method thereof.

Background technique

Chemical industry includes organic chemical industry and inorganic chemical industry. There are various chemical products with complex components. The wastewater discharged from chemical plants is called chemical wastewater. There are many kinds of chemical wastewater, most of which are highly toxic and not easy to purify. They have a certain accumulation in organisms and have obvious oxygen-consuming properties in water bodies, which can easily deteriorate water quality.

The water quality composition of chemical wastewater is complex, the water quality composition is complex, and there are many by-products. The reaction raw materials are often solvent-like substances or compounds with ring structures, which increases the difficulty of wastewater treatment. Due to the incomplete reaction of raw materials and the large amount of solvent medium used in raw materials or production entering the wastewater system, the pollutant content in wastewater is very high. Moreover, there are many toxic and harmful substances in chemical wastewater, and many organic pollutants in fine chemical wastewater are toxic and harmful to microorganisms. Such as halogen compounds, nitro compounds, dispersants or surfactants with bactericidal effect, etc. Not only that, there are many biodegradable substances in chemical wastewater, poor biodegradability, and high chroma of wastewater.

Because chemical wastewater pollutes the environment very much, it is very necessary to treat chemical wastewater. The production cost of existing products is relatively high, which is not conducive to comprehensive promotion and application. In today's chemical wastewater treatment industry, the water quality is becoming more and more complex, and the requirements for water treatment chemicals are also increasing. At present, polyacrylamide, a polymer flocculant commonly used in the market, adopts a relatively single monomer structure, and the product has a narrow application area, which cannot meet the requirements of different water quality in different industries.

Contents of the invention

The object of the present invention is to provide a kind of broad-spectrum high, good stability flocculant for chemical wastewater and its preparation method, to solve the problems raised in the above-mentioned background technology.

To achieve the above object, the present invention provides the following technical solutions:

A flocculant for chemical waste water, raw materials according to parts by weight include: 20-30 parts of non-ionic monomers, 3-5 parts of anionic monomers, 10-20 parts of cationic monomers, dimethylaminoethyl methacrylate monomer 2-4 parts, 0.05-0.09 parts of initiator, 0.3-0.5 parts of ammonium persulfate, 120-140 parts of deionized water, 20-40 parts of fly ash.

As a further solution of the present invention: the flocculant for chemical wastewater, raw materials in parts by weight include: 22-28 parts of nonionic monomers, 3.5-4.5 parts of anionic monomers, 12-18 parts of cationic monomers, methacrylic acid 2.5-3.5 parts of dimethylaminoethyl ester monomer, 0.06-0.08 parts of initiator, 0.35-0.45 parts of ammonium persulfate, 125-135 parts of deionized water, and 25-35 parts of fly ash.

As a further solution of the present invention: the flocculant for chemical waste water, raw materials according to parts by weight include: 25 parts of nonionic monomers, 4 parts of anionic monomers, 15 parts of cationic monomers, dimethylaminoethyl methacrylate mono 3 parts of body, 0.07 parts of initiator, 0.4 parts of ammonium persulfate, 130 parts of deionized water, and 30 parts of fly ash.

As a further solution of the present invention: the non-ionic monomers are acrylamide, methacrylamide and nitrogen substitutes thereof.

As a further solution of the present invention: the cationic monomer is acryloyloxyethyltrimethylammonium chloride, methacryloyloxyethyltrimethylammonium chloride or a combination of both.

As a further solution of the present invention: the anionic monomer is one or more of sodium acrylate, sodium 2-acryloyl-2-methylpropanesulfonate and acryloyl morpholine.

As a further solution of the present invention: the initiator is a redox initiator, a water-soluble azo initiator or a combination of the two.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment and treat at 40-80°C for 1-3 hours to obtain modified fly ash. The weight concentration of hydrochloric acid solution is 32-36%, and the amount of hydrochloric acid solution is sufficient Wet the fly ash, the ultrasonic frequency is 60-80KHz, and the power density is 50-70w/L. This operation can greatly improve the stability of the product, which can increase the product stability by 20%-30%;

(3) Place the dimethylaminoethyl methacrylate monomer at 50-70°C and a negative pressure of 0.094-0.098MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate In the monomer, and obtain the quaternization monomer;

(4) Add nonionic monomers, anionic monomers, cationic monomers, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence, control the starting temperature at 35-45°C, and stir at a speed of 500-600rpm 10-20min, during the stirring process, the temperature is increased by 1°C-2°C per minute, after the stirring is over, let it stand for 5-10min, the initial temperature is controlled at 35-45°C and then stirred at a speed of 500-600rpm for 10- For 20 minutes, the temperature decreases at a rate of 1°C-2°C per minute, and then stands still for 5-10 minutes. Finally, nitrogen gas is blown in to remove dissolved oxygen, and finally an initiator is added for polymerization reaction. Through the above operations, the effect of polymerization reaction can be better improved, compared The current level should be increased by 15%-20%. On the other hand, it is also beneficial to improve the stability of the product, so that the stability of the product can be further improved;

(5) After the polymerization reaction is carried out for 3-4 hours, add the treated modified fly ash and continue the reaction for 4-6 hours to obtain an emulsion, then add sodium hydroxide to the emulsion to adjust the pH value of the emulsion to 5.5-6, Then continue to stir at 700-900rpm for 20-30 minutes to obtain the finished flocculant. The whole finished product has a simple production process and low production cost. If it is widely used, it can save the country's economic expenditure by 100-100 million yuan every year.

Compared with prior art, the beneficial effect of the present invention is:

The present invention has a higher density of charged groups, stronger adsorption and capture ability for colloids and suspended particles in water, high temperature resistance, high salt resistance, acid and alkali resistance, high broad spectrum and good stability compared with other flocculants. The flocculation effect is good. When used in sewage treatment, it has higher decolorization effect and higher DOD removal effect, and achieves the comprehensive treatment effect of sewage, which not only enhances the effect of chemical treatment of sewage, but also makes fly ash become waste. The treasure has been comprehensively utilized, and the production cost of the product is relatively low, which meets the needs of the country and is suitable for comprehensive promotion and application.

detailed description

The technical solution of this patent will be further described in detail below in conjunction with specific embodiments.

Example 1

A flocculant for chemical waste water, the raw materials according to parts by weight include: 20 parts of nonionic monomers, 3 parts of anionic monomers, 10 parts of cationic monomers, 2 parts of dimethylaminoethyl methacrylate monomers, 0.05 parts of initiator parts, 0.3 parts of ammonium persulfate, 120 parts of deionized water, and 20 parts of fly ash.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment, and treat at 40°C for 1 hour to obtain modified fly ash. The weight concentration of the hydrochloric acid solution is 32%, and the amount of hydrochloric acid solution is enough to wet the fly ash. Ultrasonic frequency is 60KHz, power density is 50w/L;

(3) Place the dimethylaminoethyl methacrylate monomer at 50°C and a negative pressure of 0.094MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate monomer, And obtain the quaternization monomer;

(4) Add the non-ionic monomer, anionic monomer, cationic monomer, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence. During the process, the temperature increased at 2°C per minute. After the stirring was completed, it was left to stand for 5 minutes. The temperature was controlled at 45°C and then stirred at a speed of 500 rpm for 10 minutes. The temperature was decreased at 2°C per minute, and then stood for 5 minutes. Nitrogen is blown in to remove dissolved oxygen, and finally an initiator is added for polymerization;

(5) After the polymerization reaction was carried out for 3 hours, the treated modified fly ash was added, and the reaction was continued for 4 hours to obtain an emulsion, and then sodium hydroxide was added to the emulsion to adjust the pH value of the emulsion to 5.5, and then continue at a speed of 700rpm Stir for 20 minutes to obtain the finished flocculant.

Example 2

A flocculant for chemical waste water, the raw materials according to weight parts include: 22 parts of nonionic monomers, 3.5 parts of anionic monomers, 12 parts of cationic monomers, 2.5 parts of dimethylaminoethyl methacrylate monomers, 0.06 parts of initiators parts, 0.35 parts of ammonium persulfate, 125 parts of deionized water, and 25 parts of fly ash.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment, and treat at 50°C for 1.5 hours to obtain modified fly ash. The weight concentration of the hydrochloric acid solution is 33%, and the amount of hydrochloric acid solution is enough to wet the fly ash , the ultrasonic frequency is 65KHz, and the power density is 55w/L;

(3) Place the dimethylaminoethyl methacrylate monomer at 55°C and a negative pressure of 0.095MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate monomer, And obtain the quaternization monomer;

(4) Add the non-ionic monomer, anionic monomer, cationic monomer, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence. During the process, the temperature was increased by 2°C per minute. After the stirring was completed, it was left to stand for 5 minutes. The temperature was controlled at 45°C and then stirred at a speed of 520 rpm for 12 minutes. The temperature was decreased by 2°C per minute, and then stood for 5 minutes. Nitrogen is blown in to remove dissolved oxygen, and finally an initiator is added for polymerization;

(5) After the polymerization reaction was carried out for 3.2 hours, the treated modified fly ash was added, and the reaction was continued for 4.5 hours to obtain an emulsion, and then sodium hydroxide was added to the emulsion to adjust the pH value of the emulsion to 5.6, and then the 750rpm The rotation speed continued to stir for 22 minutes to obtain the finished flocculant.

Example 3

A flocculant for chemical waste water, the raw materials according to parts by weight include: 25 parts of nonionic monomers, 4 parts of anionic monomers, 15 parts of cationic monomers, 3 parts of dimethylaminoethyl methacrylate monomers, 0.07 parts of initiator parts, 0.4 parts of ammonium persulfate, 130 parts of deionized water, and 30 parts of fly ash.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment, and treat at 60°C for 2 hours to obtain modified fly ash. The weight concentration of the hydrochloric acid solution is 34%, and the amount of hydrochloric acid solution is enough to wet the fly ash. Ultrasonic frequency is 70KHz, power density is 60w/L;

(3) Place the dimethylaminoethyl methacrylate monomer at 60°C and a negative pressure of 0.096MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate monomer, And obtain the quaternization monomer;

(4) Add the non-ionic monomer, anionic monomer, cationic monomer, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence. During the process, the temperature increases at 1.5°C per minute. After the stirring is completed, it is left to stand for 7.5 minutes. The temperature is controlled at 40°C and then stirred at a speed of 550rpm for 15 minutes. The temperature is gradually decreased at 1.5°C per minute. Finally, nitrogen is blown in to remove dissolved oxygen, and finally an initiator is added for polymerization;

(5) After the polymerization reaction is carried out for 3.5 hours, add the treated modified fly ash, continue to react for 5 hours to obtain an emulsion, then add sodium hydroxide to the emulsion, adjust the pH value of the emulsion to 5.8, and then rotate at 800rpm Continue to stir for 25 minutes to obtain the finished flocculant.

Example 4

A flocculant for chemical waste water, the raw materials according to weight parts include: 28 parts of nonionic monomers, 4.5 parts of anionic monomers, 18 parts of cationic monomers, 3.5 parts of dimethylaminoethyl methacrylate monomers, 0.08 parts of initiator parts, 0.45 parts of ammonium persulfate, 135 parts of deionized water, and 35 parts of fly ash.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment, and treat at 70°C for 2.5 hours to obtain modified fly ash. The weight concentration of the hydrochloric acid solution is 35%, and the amount of hydrochloric acid solution is enough to wet the fly ash , the ultrasonic frequency is 75KHz, and the power density is 65w/L;

(3) Place the dimethylaminoethyl methacrylate monomer at 65°C and a negative pressure of 0.097MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate monomer, And obtain the quaternization monomer;

(4) Add the nonionic monomer, anionic monomer, cationic monomer, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence, control the temperature at 45°C, stir at 600rpm for 20min, and During the process, the temperature is increased at 1°C per minute. After the stirring is completed, let it stand still for 10 minutes. The temperature is controlled at 45°C and then stirred at a speed of 600rpm for 20 minutes. Nitrogen is used to remove dissolved oxygen, and finally an initiator is added for polymerization;

(5) After the polymerization reaction was carried out for 3.8 hours, the treated modified fly ash was added, and the reaction was continued for 5.5 hours to obtain an emulsion, and then sodium hydroxide was added to the emulsion to adjust the pH value of the emulsion to 5.9, and then the 850rpm The rotation speed continued to stir for 28 minutes to obtain the finished flocculant.

Example 5

A flocculant for chemical waste water, the raw materials according to weight parts include: 30 parts of nonionic monomers, 5 parts of anionic monomers, 20 parts of cationic monomers, 4 parts of dimethylaminoethyl methacrylate monomers, 0.09 parts of initiator parts, 0.5 parts of ammonium persulfate, 140 parts of deionized water, and 40 parts of fly ash.

The preparation method of described chemical industry wastewater flocculant, concrete steps are as follows:

(1) Weigh each raw material according to parts by weight;

(2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment, and treat at 80°C for 3 hours to obtain modified fly ash. The weight concentration of hydrochloric acid solution is 36%, and the amount of hydrochloric acid solution is enough to wet the fly ash. Ultrasonic frequency is 80KHz, power density is 70w/L;

(3) Place the dimethylaminoethyl methacrylate monomer at 70°C and a negative pressure of 0.098MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate monomer, And obtain the quaternization monomer;

(4) Add the non-ionic monomer, anionic monomer, cationic monomer, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence. During the process, the temperature was increased by 2°C per minute. After the stirring was completed, it was left to stand for 10 minutes. The temperature was controlled at 45°C and stirred at a speed of 600 rpm for 20 minutes. The temperature was decreased by 2°C per minute, and then stood for 5 minutes. Nitrogen is blown in to remove dissolved oxygen, and finally an initiator is added for polymerization;

(5) After the polymerization reaction was carried out for 4 hours, the treated modified fly ash was added, and the reaction was continued for 6 hours to obtain an emulsion, and then sodium hydroxide was added to the emulsion to adjust the pH value of the emulsion to 6, and then continue at a speed of 900rpm Stir for 30 minutes to obtain the finished flocculant.

The nonionic monomers are acrylamide, methacrylamide and nitrogen substitutes thereof; the cationic monomers are acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl chloride ammonium chloride or a combination of the two; the anionic monomer is one or more of sodium acrylate, sodium 2-acryloyl-2-methylpropanesulfonate and acryloyl morpholine; the initiator is Redox initiators, water-soluble azo initiators or a combination of both.

The present invention has a higher density of charged groups, stronger adsorption and capture ability for colloids and suspended particles in water, high temperature resistance, high salt resistance, acid and alkali resistance, high broad spectrum and good stability compared with other flocculants. The characteristics of good flocculation effect, when used in sewage treatment, have higher decolorization effect and higher DOD removal effect, to achieve the overall treatment effect of sewage, that is, to enhance the effect of chemical treatment of sewage, and to turn fly ash into waste Treasures have been comprehensively utilized.

The preferred implementation of this patent has been described in detail above, but this patent is not limited to the above-mentioned implementation. Within the scope of knowledge possessed by those of ordinary skill in the art, various modifications can be made without departing from the purpose of this patent. kind of change.

Claims (8)

1. A flocculant for chemical waste water is characterized in that, the raw materials according to weight parts include: 20-30 parts of nonionic monomers, 3-5 parts of anionic monomers, 10-20 parts of cationic monomers, dimethacrylic acid 2-4 parts of methyl amino ethyl ester monomer, 0.05-0.09 parts of initiator, 0.3-0.5 parts of ammonium persulfate, 120-140 parts of deionized water, and 20-40 parts of fly ash. 2. The flocculant for chemical waste water according to claim 1, characterized in that, the raw materials in parts by weight include: 22-28 parts of nonionic monomers, 3.5-4.5 parts of anionic monomers, 12-18 parts of cationic monomers , 2.5-3.5 parts of dimethylaminoethyl methacrylate monomer, 0.06-0.08 parts of initiator, 0.35-0.45 parts of ammonium persulfate, 125-135 parts of deionized water, and 25-35 parts of fly ash. 3. The flocculant for chemical waste water according to claim 1 is characterized in that, the raw materials according to parts by weight include: 25 parts of nonionic monomers, 4 parts of anionic monomers, 15 parts of cationic monomers, dimethyl methacrylate 3 parts of aminoethyl ester monomer, 0.07 part of initiator, 0.4 part of ammonium persulfate, 130 parts of deionized water, 30 parts of fly ash. 4. The flocculant for chemical wastewater according to any one of claims 1-3, wherein the nonionic monomer is acrylamide, methacrylamide and nitrogen substitutes thereof. 5. The flocculant for chemical wastewater according to any one of claims 1-3, wherein the cationic monomer is acryloyloxyethyltrimethylammonium chloride, methacryloyloxyethyltrimethylammonium ammonium chloride or a combination of the two. 6. The flocculant for chemical wastewater according to any one of claims 1-3, characterized in that, the anionic monomer is sodium acrylate, 2-acryloyl-2-sodium methylpropanesulfonate and acryloylmorpholine one or more of them. 7. The flocculant for chemical wastewater according to any one of claims 1-3, wherein the initiator is a redox initiator, a water-soluble azo initiator or a combination of the two. 8. A preparation method of a flocculant for chemical waste water as claimed in any one of claims 1-3, characterized in that, the specific steps are as follows: (1) Weigh each raw material according to parts by weight; (2) Mix fly ash and hydrochloric acid solution in an ultrasonic environment and treat at 40-80°C for 1-3 hours to obtain modified fly ash. The weight concentration of hydrochloric acid solution is 32-36%, and the amount of hydrochloric acid solution is sufficient Wet the fly ash, the ultrasonic frequency is 60-80KHz, and the power density is 50-70w/L; (3) Place the dimethylaminoethyl methacrylate monomer at 50-70°C and a negative pressure of 0.094-0.098MPa for distillation and purification, and add the quaternization reagent to the purified dimethylaminoethyl methacrylate In the monomer, and obtain the quaternization monomer; (4) Add nonionic monomers, anionic monomers, cationic monomers, ammonium persulfate and deionized water into the reaction kettle of the vacuum disperser in sequence, control the starting temperature at 35-45°C, and stir at a speed of 500-600rpm 10-20min, during the stirring process, the temperature is increased by 1°C-2°C per minute, after the stirring is over, let it stand for 5-10min, the initial temperature is controlled at 35-45°C and then stirred at a speed of 500-600rpm for 10- For 20 minutes, the temperature decreases at a rate of 1°C-2°C per minute, and then stands still for 5-10 minutes, and finally blows nitrogen gas to remove dissolved oxygen, and finally adds an initiator to carry out polymerization reaction; (5) After the polymerization reaction is carried out for 3-4 hours, add the treated modified fly ash and continue the reaction for 4-6 hours to obtain an emulsion, then add sodium hydroxide to the emulsion to adjust the pH value of the emulsion to 5.5-6, Then continue to stir for 20-30min at the speed of 700-900rpm to obtain the finished flocculant.