CN113845193A - Preparation method of efficient coagulant - Google Patents

Preparation method of efficient coagulant Download PDF

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Publication number
CN113845193A
CN113845193A CN202111293370.5A CN202111293370A CN113845193A CN 113845193 A CN113845193 A CN 113845193A CN 202111293370 A CN202111293370 A CN 202111293370A CN 113845193 A CN113845193 A CN 113845193A
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Prior art keywords
coagulant
preparation
emulsion stabilizer
main agent
agent
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CN202111293370.5A
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Inventor
丁国际
周婷
魏婉蓉
唐量
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN202111293370.5A priority Critical patent/CN113845193A/en
Publication of CN113845193A publication Critical patent/CN113845193A/en
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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
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • 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
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention discloses a preparation method of a high-efficiency coagulant, which comprises the following components in percentage by weight: 20-40% of coagulant main agent, 20-60% of deionized water, 20-40% of settling agent and 1-8% of emulsion stabilizer. The preparation method can improve the coagulation effect and the universality; the addition of the emulsion stabilizer enables the settling agent to be uniformly mixed with the coagulant main agent, so that the coagulation speed is accelerated; in addition, the preparation method is simple, convenient to use, large in generated floc, high in settling speed and good in treatment effect when used for treating high-concentration organic wastewater difficult to degrade.

Description

Preparation method of efficient coagulant
Technical Field
The invention relates to the technical field of preparation of efficient coagulants, in particular to a preparation method of an efficient coagulant.
Background
The coagulation treatment method is a common method for water treatment, and colloidal matter, organic matter, and the like in water can be removed by coagulation treatment. Coagulants used in water treatment are often classified into inorganic coagulants and organic coagulants. Compared with inorganic coagulant, organic coagulant has the advantages of less consumption, wide water quality adaptation range, high flocculation speed and the like, so that the organic coagulant is more and more widely applied in China.
The organic coagulant is natural or artificial organic molecular substance capable of generating flocculation. The natural product is protein or polysaccharide compound, such as chitosan extracted from crustacean of marine arthropod such as shrimp and crab, insect crustacean, mollusk shell and skeleton, and cell wall of higher plant. The artificial synthetic products include polyacrylamide, polyamine coagulant, etc. Different organic coagulants have different coagulation effects.
However, in order to obtain better treatment effect in water treatment, two or more organic coagulants are often needed to be used simultaneously, but different types of organic coagulants are inconvenient to be added and used respectively. For example, in patent CN 111592082A, a paint mist coagulant synthesized for treating paint wastewater is developed, and the paint mist coagulant consists of agent a and agent B. When in use, the agent A and the agent B need to be added respectively, thus increasing the complexity of the operation. In addition, one problem that is common in the use of organic coagulants is that the flocs formed by the organic coagulants are slow and are in a state of neither completely sinking nor completely floating, so that the gravity separation of the flocs from liquid is not facilitated, and the coagulation effect is seriously influenced. Therefore, the technical problem to be solved by the invention is to provide a preparation method of a high-efficiency coagulant which can combine a plurality of organic matters into a whole, has high floc formation speed and is easy for solid-liquid gravity separation and can be used for treating refractory organic wastewater.
Disclosure of Invention
The invention aims to provide a preparation method of a high-efficiency coagulant, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the high-efficiency coagulant comprises the following components in percentage by weight: 20-40% of coagulant main agent, 20-60% of deionized water, 20-40% of settling agent and 1-8% of emulsion stabilizer.
Preferably, the preparation method of the high-efficiency coagulant comprises the following steps:
A. sequentially adding 10-20 ml of dimethyl diallyl ammonium chloride, 10-20 g of acrylamide and 45-75 ml of pure water into a reaction kettle;
B. after dissolving, respectively adding 0.002-0.008 g of EDTA-2Na, 0.005-0.01 g of isopropanol and 0.005-0.001 g of urea, introducing nitrogen at 35 ℃ for 30-40 min, adding 0.01-0.05 g of ammonium persulfate, and reacting for 10 min;
C. then adding 0.003-0.006 g of sodium bisulfite, and continuously keeping the temperature at 35 ℃ for reaction for 0.5-2 h;
D. adjusting the temperature to 60 ℃, adding 0.1-1 g of chitosan, and continuing to react for 0.5-3 h to obtain the main agent.
Preferably, the settling agent is one or more of modified diatomite, modified kaolin and the like.
Preferably, the modified diatomite is particles with the particle size of less than 50 μm, which are obtained by properly crushing natural diatomite, treating the natural diatomite for 5-30 min under the microwave power of 320W and sieving the natural diatomite; the modified kaolin refers to particles with the particle size of less than 50 mu m, which are obtained by properly crushing natural kaolin, processing the crushed natural kaolin for 5-30 min under the microwave power of 320W and sieving the crushed natural kaolin.
Preferably, the emulsion stabilizer is sodium carboxymethylcellulose.
Preferably, the preparation method of the emulsion stabilizer sodium carboxymethylcellulose comprises the following steps: 0.1-1 g of sodium carboxymethylcellulose is weighed, dissolved in 100ml of deionized water and stirred uniformly.
Preferably, the preparation method comprises the following steps: adding a main agent and deionized water in a reaction kettle according to weight percentage respectively, and uniformly stirring; then adding the settling agent and the emulsion stabilizer respectively according to the weight percentage under stirring, and obtaining the finished product of the high-efficiency coagulant after uniform stirring.
Compared with the prior art, the invention has the beneficial effects that:
(1) aiming at the problems that the coagulation effect is limited when a single organic coagulant is used for treating wastewater by using a coagulation method, and even some single organic coagulants need to be added step by step to cause complicated implementation steps, the invention not only improves the coagulation effect and the universality, but also simplifies the operation process of adding the coagulants and saves related coagulation equipment by compounding natural organic matters and artificially synthesized organic matters into 1 kind of coagulants.
(2) Aiming at the problems that flocs formed by an organic coagulant often cannot completely sink or float and are not beneficial to separation of the flocs from liquid, the invention enables an inorganic settling aid to be well integrated with a coagulant main agent by using an emulsion stabilizer, so that the coagulant can quickly form compact flocs and well settle after being added with wastewater, thereby being beneficial to solid-liquid separation of the flocs from the liquid.
(3) The preparation method of the high-efficiency coagulant provided by the invention is easy, the prepared high-efficiency coagulant is composed of a plurality of organic matters, has wide adaptability, and particularly has good coagulation removal effect on the organic matters of high-concentration organic wastewater. In practical application, only one-time addition of the efficient coagulant is needed, so that manpower and material resources are saved, and the method has outstanding environmental benefits and economic benefits.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides the following technical scheme: the high-efficiency coagulant comprises the following components in percentage by weight: 20-40% of coagulant main agent, 20-60% of deionized water, 20-40% of settling agent and 1-8% of emulsion stabilizer.
The first embodiment is as follows:
in this example, coagulant a and coagulant B were prepared separately for comparison of the effect of the settling agent. The coagulation treatment object is coking wastewater.
The preparation method of the coagulant comprises the following steps:
1) preparing a coagulant main agent: sequentially adding 20ml of dimethyl diallyl ammonium chloride, 12.6g of acrylamide and 63.8ml of pure water into a reaction kettle, respectively adding 0.003g of EDTA-2Na, 0.006g of isopropanol and 0.001g of urea after dissolution, introducing nitrogen at 35 ℃ for 30min, adding 0.012g of ammonium persulfate to react for 10min, then adding 0.003g of sodium bisulfite, and continuously keeping at 35 ℃ to react for 1.5 h; adjusting the temperature to 60 ℃, adding 0.5g of chitosan, and continuously reacting for 1.5h to obtain a coagulant main agent;
2) preparing a settling agent: the settling agent is modified diatomite. The modified diatomite is particles with particle size less than 50 μm obtained by mechanically pulverizing natural diatomite, treating under microwave power of 320W for 10min, and sieving;
3) preparing an emulsion stabilizer: the emulsion stabilizer comprises sodium carboxymethylcellulose. Weighing 1g of sodium carboxymethylcellulose, dissolving in 100ml of deionized water, and uniformly stirring;
4) preparation of a coagulant A: adding 20 weight percent of coagulant main agent and 58 weight percent of deionized water into a reaction kettle at normal temperature, and uniformly stirring; adding 20 percent by weight of settling agent and 3 percent by weight of emulsion stabilizer under stirring, and preparing the high-efficiency coagulant after uniformly stirring; .
5) Preparation of coagulant B: adding 20 percent by weight of coagulant main agent and 58 percent by weight of deionized water into a reaction kettle at normal temperature, and uniformly stirring.
Adding 10L of coking wastewater into the coagulation reactor A, and starting a stirrer at a stirring speed of 200 r/min; then adding 10mL of coagulant A into the coagulation reactor, and quickly stirring for 30 s; adjusting the stirring speed to 40r/min, stirring for 15min at a low speed, closing the stirrer, sampling and observing the floc formation condition.
Adding 10L of coking wastewater into the coagulation reactor B, and starting a stirrer at a stirring speed of 200 r/min; then adding a coagulant B with the same amount as the main agent of the coagulant A into the coagulation reactor, and quickly stirring for 30 seconds; adjusting the stirring speed to 40r/min, stirring for 15min at a low speed, closing the stirrer, sampling and observing the floc formation condition.
The floc formed by the coagulant A containing the settling agent completely sinks under the action of gravity, is easy for solid-liquid separation and has good coagulating sedimentation effect. The floc formed by the coagulant B without the settling agent is in a suspension state and is not completely precipitated or floated, so that the solid-liquid separation cannot be simply realized by adopting a gravity method. The main agent and the settling agent of the composite organic coagulant obviously improve the density and the settleability of flocs.
Example two:
the coagulant preparation procedure of this example is substantially the same as the coagulant a preparation procedure of example one, and is characterized in that:
1) preparing a coagulant main agent: sequentially adding 16.5ml of dimethyl diallyl ammonium chloride, 10.1g of acrylamide and 73.4ml of pure water into a reaction kettle, respectively adding 0.003g of EDTA-2Na, 0.006g of isopropanol and 0.001g of urea after dissolution, introducing nitrogen at 35 ℃ for 35min, adding 0.012g of ammonium persulfate to react for 10min, then adding 0.003g of sodium bisulfite, and continuously keeping at 35 ℃ to react for 1.5 h; adjusting the temperature to 60 ℃, adding 0.2g of chitosan, and continuously reacting for 1.5h to obtain a coagulant main agent;
2) preparing a settling agent: the settling agent is modified diatomite. The modified diatomite is particles with particle size less than 50 μm obtained by mechanically pulverizing natural diatomite, treating under microwave power of 320W for 10min, and sieving;
3) preparing an emulsion stabilizer: the emulsion stabilizer comprises sodium carboxymethylcellulose. Weighing 1g of sodium carboxymethylcellulose, dissolving in 100ml of deionized water, and uniformly stirring;
4) preparing a coagulant: adding 30 weight percent of coagulant main agent and 45 weight percent of deionized water into a reaction kettle at normal temperature, and uniformly stirring; adding 20 percent by weight of settling agent and 5 percent by weight of emulsion stabilizer under stirring, and finally preparing the high-efficiency coagulant after uniformly stirring.
In this example, the object of coagulation treatment was coating wastewater, and the COD concentration of the wastewater was 3050 mg/L. Adding 10L of wastewater into the coagulation reactor, and starting a stirrer at a stirring speed of 200 r/min; then 10mL of the coagulant is added into the coagulation reactor, and the mixture is rapidly stirred for 30 s; adjusting the stirring speed to 40r/min, stirring for 15min at a low speed, closing the stirrer, standing for 10min, sampling and analyzing the COD concentration and the ammonia nitrogen concentration in the liquid, wherein the COD concentration after treatment is 460 mg/L.
Example three:
the coagulant preparation procedure of this example is substantially the same as the coagulant a preparation procedure of example one, and is characterized in that:
1) preparing a coagulant main agent: sequentially adding 18.5ml of dimethyldiallylammonium chloride, 11.2g of acrylamide and 70.3ml of pure water into a reaction kettle, respectively adding 0.003g of EDTA-2Na, 0.005g of isopropanol and 0.001g of urea after dissolution, introducing nitrogen at 35 ℃ for 30-40 min, adding 0.012g of ammonium persulfate to react for 10min, then adding 0.003g of sodium bisulfite, and continuously keeping at 35 ℃ to react for 1.5 h; adjusting the temperature to 60 ℃, adding 0.1g of chitosan, and continuously reacting for 1.5h to obtain a coagulant main agent;
2) preparing a settling agent: the settling agent is modified diatomite. The modified diatomite is particles with particle size less than 50 μm obtained by mechanically pulverizing natural diatomite, treating under microwave power of 320W for 10min, and sieving.
3) Preparing an emulsion stabilizer: the emulsion stabilizer comprises sodium carboxymethylcellulose. 1g of sodium carboxymethylcellulose is weighed out and dissolved in 100ml of deionized water and stirred uniformly.
4) Preparing a coagulant: adding 30 weight percent of coagulant main agent and 45 weight percent of deionized water into a reaction kettle at normal temperature, and uniformly stirring; adding 20 percent by weight of settling agent and 5 percent by weight of emulsion stabilizer under stirring, and finally preparing the high-efficiency coagulant after uniformly stirring.
In conclusion, in the present embodiment, the coagulation treatment object is the water-based paint wastewater, the COD concentration of the wastewater is 3110mg/L, and the turbidity is 804 NTU. Adding 10L of wastewater into the coagulation reactor, and starting a stirrer at a stirring speed of 200 r/min; then 5mL of the coagulant is added into the coagulation reactor, and the mixture is rapidly stirred for 30 s; adjusting the stirring speed to 30r/min, stirring slowly for 15min, closing the stirrer, standing for 10min, sampling and analyzing the COD concentration and turbidity in the liquid, wherein the COD concentration is 410mg/L and the turbidity is 31NTU after treatment; aiming at the problems that the coagulation effect is limited when a single organic coagulant is used for treating wastewater by using a coagulation method, and even some single organic coagulants need to be added step by step to cause complex implementation steps, the invention not only improves the coagulation effect and the universality, but also simplifies the coagulant adding operation process and saves related coagulation equipment by compounding natural organic matters and artificially synthesized organic matters into 1 kind of coagulants; aiming at the problems that flocs formed by an organic coagulant often cannot completely sink or float and are not beneficial to separation of the flocs from liquid, the invention enables an inorganic settling aid to be well integrated with a coagulant main agent by using an emulsion stabilizer, so that the coagulant can quickly form compact flocs and well settle after being added with wastewater, thereby being beneficial to solid-liquid separation of the flocs from the liquid.
The preparation method of the high-efficiency coagulant provided by the invention is easy, the prepared high-efficiency coagulant is composed of a plurality of organic matters, has wide adaptability, and particularly has good coagulation removal effect on the organic matters of high-concentration organic wastewater. In practical application, only one-time addition of the efficient coagulant is needed, so that manpower and material resources are saved, and the method has outstanding environmental and economic benefits
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. An efficient coagulant is characterized in that: the high-efficiency coagulant comprises the following components in percentage by weight: 20-40% of coagulant main agent, 20-60% of deionized water, 20-40% of settling agent and 1-8% of emulsion stabilizer.
2. The preparation method of the high-efficiency coagulant is characterized by comprising the following steps: the preparation method of the coagulant main agent comprises the following steps:
A. sequentially adding 10-20 ml of dimethyl diallyl ammonium chloride, 10-20 g of acrylamide and 45-75 ml of pure water into a reaction kettle;
B. after dissolving, respectively adding 0.002-0.008 g of EDTA-2Na, 0.005-0.01 g of isopropanol and 0.005-0.001 g of urea, introducing nitrogen at 35 ℃ for 30-40 min, adding 0.01-0.05 g of ammonium persulfate, and reacting for 10 min;
C. then adding 0.003-0.006 g of sodium bisulfite, and continuously keeping the temperature at 35 ℃ for reaction for 0.5-2 h;
D. adjusting the temperature to 60 ℃, adding 0.1-1 g of chitosan, and continuing to react for 0.5-3 h to obtain the main agent.
3. A high efficiency coagulant as claimed in claim 1 wherein: the settling agent is one or more of modified diatomite, modified kaolin and the like.
4. A high efficiency coagulant as claimed in claim 3 wherein: the modified diatomite is particles with the particle size of less than 50 microns, which are obtained by properly crushing natural diatomite, treating the natural diatomite for 5-30 min under the microwave power of 320W and sieving the natural diatomite; the modified kaolin refers to particles with the particle size of less than 50 mu m, which are obtained by properly crushing natural kaolin, processing the crushed natural kaolin for 5-30 min under the microwave power of 320W and sieving the crushed natural kaolin.
5. A high efficiency coagulant as claimed in claim 1 wherein: the emulsion stabilizer is sodium carboxymethylcellulose.
6. A high efficiency coagulant as claimed in claim 5 wherein: the preparation method of the emulsion stabilizer sodium carboxymethylcellulose comprises the following steps: 0.1-1 g of sodium carboxymethylcellulose is weighed, dissolved in 100ml of deionized water and stirred uniformly.
7. The preparation method of the high-efficiency coagulant according to claim 1 is characterized by comprising the following steps: the preparation method comprises the following steps: adding a main agent and deionized water in a reaction kettle according to weight percentage respectively, and uniformly stirring; then adding the settling agent and the emulsion stabilizer respectively according to the weight percentage under stirring, and obtaining the finished product of the high-efficiency coagulant after uniform stirring.
CN202111293370.5A 2021-11-03 2021-11-03 Preparation method of efficient coagulant Pending CN113845193A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114477399A (en) * 2022-02-09 2022-05-13 上海大学 Composite coagulant and preparation method thereof

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CN110436553A (en) * 2019-08-23 2019-11-12 河南亿群环保科技有限公司 A kind of polyacrylamide sewage water inorganic agent and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1654497A (en) * 2005-01-14 2005-08-17 华南理工大学 Chitosan graft ternary polymerization polymeric flocculant and its preparation method and use
CN102477125A (en) * 2010-11-22 2012-05-30 袁连海 Synthesis technology of hydrophobic polymeric flocculant
CN110436553A (en) * 2019-08-23 2019-11-12 河南亿群环保科技有限公司 A kind of polyacrylamide sewage water inorganic agent and preparation method thereof

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Title
张增志等, 电子科技大学出版社 *
程建华: "壳聚糖接枝高分子絮凝剂制备及处理造纸废水研究" *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114477399A (en) * 2022-02-09 2022-05-13 上海大学 Composite coagulant and preparation method thereof

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