CN115417949B - Liquid organic sludge dehydrating agent and preparation method thereof - Google Patents
Liquid organic sludge dehydrating agent and preparation method thereof Download PDFInfo
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- CN115417949B CN115417949B CN202211365155.6A CN202211365155A CN115417949B CN 115417949 B CN115417949 B CN 115417949B CN 202211365155 A CN202211365155 A CN 202211365155A CN 115417949 B CN115417949 B CN 115417949B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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
- C02F11/00—Treatment of sludge; Devices therefor
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/148—Combined use of inorganic and organic substances, being added in the same treatment step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
Abstract
The invention discloses a liquid organic sludge dehydrating agent and a preparation method thereof, belonging to the field of preparation of high molecular polymers. The invention adds the active auxiliary monomer into the polymer monomer to be a multifunctional organic molecule, and the functional group of the multifunctional organic molecule comprises a carbon-carbon double bond and a morpholine group. Due to the addition of the functional monomers, a morpholine group is arranged on a branched chain of the cationic polymer, the cationic polymer is of a six-membered ring structure, and the number of receptors of hydrogen bonds is two, so that double hydrogen bonds can be formed in molecules, the high molecular polymer is shrunk to a certain extent, the high molecular polymer has good fluidity under the state of aqueous solution with certain molecular weight, the viscosity of the high molecular polymer can be reduced on the basis of the same molecular weight, and meanwhile, in sludge dewatering, the high molecular polymer can well carry water in sludge due to the special structure, so that the sludge settling rate is increased, and the high molecular polymer has the advantages of strong filterability and high dewatering rate.
Description
Technical Field
The invention belongs to the field of preparation of high molecular polymers, and particularly relates to a liquid organic sludge dehydrating agent and a preparation method thereof.
Background
With the continuous improvement of urbanization in China, the scale and population of cities are also continuously improved, urban sewage plants are also continuously built, the amount of sludge in sewage is rapidly increased, and the huge amount of sludge brings considerable pressure to the urban sewage plants, which is not only about economic and environmental problems, so that how to improve the sludge dewatering performance and improve the sludge dewatering efficiency becomes an important problem in the field of sludge treatment. Among the sludge treatment technologies of the existing acid treatment process, advanced oxidation process, freezing and thawing process, chemical conditioning process and bioleaching process, the flocculation treatment sludge process is more concerned due to the characteristics of simplicity, economy and high efficiency.
However, most of the existing flocculation processes belong to dry powder type auxiliaries, the emulsion type flocculating agent can not be directly used after long dissolving time, the requirement on equipment is high in the using process, secondary pollution is easily caused due to the fact that a system of the emulsion type flocculating agent contains a large amount of surfactants and hydrocarbon substances after the emulsion type flocculating agent is used, the aqueous solution product can be directly used, secondary pollution is not caused, and the emulsion type flocculating agent belongs to an environment-friendly product.
Most of the sludge dehydrating agents currently used in the market have the problems of complicated chemical dosing components, large dosage and the like, so that a novel liquid sludge dehydrating agent is required to be researched.
Disclosure of Invention
In order to overcome the technical defects, the invention provides a liquid organic sludge dehydrating agent and a preparation method thereof, which aim to solve the problems related to the background technology.
The invention provides a liquid organic sludge dehydrating agent and a preparation method thereof, wherein the preparation method comprises the following steps:
step 1, adding an aqueous solution of a cationic monomer into a reaction kettle, adding a functional structural monomer, adding a metal ion chelating agent, adding a chain transfer agent, stirring to completely dissolve, adjusting the pH value to 5-7, heating the temperature of the materials in the reaction kettle to 70-90 ℃, and introducing nitrogen into the reaction kettle;
step 2, respectively dripping an initiator aqueous solution and an acrylamide aqueous solution into the reaction kettle at a preset flow rate for 1-3h, and controlling the dripping of the initiator to be finished within 5-10min after the acrylamide aqueous solution; controlling the temperature of the materials in the reaction kettle to be 80-95 ℃ in the whole process; after the initiator is added, keeping the temperature of the materials in the reaction kettle at 80-90 ℃ and continuing to react for 0.5-2h;
step 3, adding a sodium bisulfite aqueous solution into the reaction kettle, and keeping the temperature of the materials in the reaction kettle between 80 and 100 ℃ to continue the reaction for 0.5 to 2 hours; cooling, when the temperature of the reaction kettle is reduced to 30-50 ℃, adding the composite bactericide into the reaction kettle, and uniformly stirring to obtain the liquid organic sludge dehydrating agent.
Preferably or alternatively, the structural functional monomer has the formula:
Wherein R1 is-CH 2 -、–CH 2 -CH 2 -、–CH 2 -CH 2 -CH 2 -one of the above; r2 is-CH 2 -、–CH 2 -CH 2 -、–CH 2 -CH 2 -CH 2 -one of the above; r3 is-CH 2 -、–CH 2 -CH 2 -、–CH 2 -CH 2 -CH 2 -one of the above.
Preferably or optionally, the cationic monomer is one or more of acryloyloxyethyltrimethyl ammonium chloride, methacryloyloxyethyltrimethyl ammonium chloride, acryloyloxyethyldimethylbenzyl ammonium chloride, methacryloyloxyethyldimethylbenzyl ammonium chloride, acryloylpropyltrimethyl ammonium chloride and dimethyldiallylammonium chloride.
Preferably or optionally, the metal ion chelating agent is one or a mixture of sodium citrate, disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, sodium gluconate and sodium tripolyphosphate.
Preferably or alternatively, the chain transfer agent is one or a mixture of sodium benzoate, sodium hypophosphite, sodium bisulfite, sodium formate, sodium acetate and n-butanol.
Preferably or optionally, the initiator is one or a mixture of potassium persulfate, sodium persulfate and ammonium persulfate.
Preferably or optionally, the composite bactericide comprises EDTA, sodium benzoate, sodium metabisulfite, sodium nitrate; and the mass ratio of each component is 2:1:1:2.
preferably or alternatively, the mass ratio of the cationic monomer to the acrylamide on a dry basis is from 1 to 1.5; the dosage of the functional structural monomer is 5-10% of the mass of the dry-based cationic monomer;
the dosage of the metal chelating agent is 0.03-0.08% of the mass of the dry-based cationic monomer; the dosage of the chain transfer agent is 0.03-0.08% of the mass of the dry-base cationic monomer; the dosage of the initiator is 0.2 to 0.8 percent of the mass of the dry-based cationic monomer; the dry basis amount of sodium bisulfite in the sodium bisulfite aqueous solution is 1 to 3 percent of the mass of dry cation monomer; the dosage of the composite bactericide is 0.2-0.5% of the mass of the dry-based cationic monomer.
The invention also provides a liquid organic sludge dehydrating agent obtained based on the preparation method of the liquid organic sludge dehydrating agent.
The invention relates to a liquid organic sludge dehydrating agent and a preparation method thereof, compared with the prior art, the liquid organic sludge dehydrating agent has the following beneficial effects: on one hand, in the selection of the polymerization monomer, the added active assistant monomer is a multifunctional organic molecule, and the functional group of the multifunctional organic molecule comprises a carbon-carbon double bond and a morpholine group. Due to the addition of the functional monomers, a morpholine group is arranged on a branched chain of the cationic polymer, the cationic polymer is of a six-membered ring structure, and the number of receptors of hydrogen bonds is two, so that double hydrogen bonds can be formed in molecules, the high molecular polymer is shrunk to a certain extent, the high molecular polymer has good fluidity under the state of aqueous solution with certain molecular weight, the viscosity of the high molecular polymer can be reduced on the basis of the same molecular weight, and meanwhile, in sludge dewatering, the high molecular polymer can well carry water in sludge due to the special structure, so that the sludge settling rate is increased, and the high molecular polymer has the advantages of strong filterability and high dewatering rate. On the other hand, the composite bactericide is added, so that the cell walls of microorganisms in water can be damaged in sludge dehydration, the polymer can conveniently and quickly enter pores of the sludge to take out water, the polymer and the water can play a synergistic effect together, water in bacteria can be effectively separated, and the purpose of deep dehydration is achieved. In addition, in the using process, the operation is simple, no other harmful medicament is added, and no secondary pollution exists.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
The invention will now be further described with reference to the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Step 1: adding 300g of 60wt% DMDAAC aqueous solution into a reaction kettle, adding 9g of N-allyl morpholine, adding 0.054g of ethylene diamine tetraacetic acid disodium and 0.054g of sodium benzoate, stirring to completely dissolve, adding sodium hydroxide or hydrochloric acid to adjust the pH value to 6.2, heating the temperature of the reaction kettle materials to 90 ℃, introducing nitrogen from the bottom of the reaction kettle for 30min, wherein the nitrogen flow rate is 60m 3 /h。
And 2, step: 36g of 1 wt% strength potassium persulfate aqueous solution and 360g of 50wt% strength acrylamide aqueous solution are respectively dripped into the reaction kettle at a certain flow rate, and the dripping of the initiator is controlled within 5min after the functional monomer and the acrylamide aqueous solution is finished. The temperature of the materials in the reaction kettle is controlled to be 90-100 ℃ in the whole process. And after the addition of the potassium persulfate aqueous solution is finished, keeping the temperature of the materials in the reaction kettle at 90-100 ℃ for 1h.
And step 3: adding 5.14g of 35wt% sodium bisulfite aqueous solution into a reaction kettle, keeping the temperature of the materials in the reaction kettle between 80 ℃ and 100 ℃ for 1h, cooling, adding 0.36g of a composite bactericide (the composite bactericide comprises EDTA, sodium benzoate, sodium metabisulfite and sodium nitrate, and the mass ratio of the components is 2.
Example 2
Step 1: 300g of a 60% strength by weight aqueous DMDAAC solution, 13.5g of N-allylmorpholine and 0.09g of disodium ethylenediaminetetraacetate were added to the reactorAdding 0.09g of sodium benzoate, stirring to completely dissolve the sodium benzoate, adding sodium hydroxide or hydrochloric acid to adjust the pH value to 6.0, heating the temperature of the materials in the reaction kettle to 90 ℃, and introducing nitrogen from the bottom of the reaction kettle for 30min, wherein the flow rate of the nitrogen is 60m 3 /h。
Step 2: 36g of 2.5 wt% potassium persulfate aqueous solution and 288g of 50wt% acrylamide aqueous solution are respectively dropwise added into the reaction kettle at a certain flow rate, and the dropwise addition of the initiator is controlled within 5min after the functional monomer and the acrylamide aqueous solution is finished. The temperature of the materials in the reaction kettle is controlled to be 90-100 ℃ in the whole process. And after the addition of the potassium persulfate aqueous solution is finished, keeping the temperature of the materials in the reaction kettle at 90-100 ℃ for 1h.
And step 3: adding 10.28g of 35wt% sodium bisulfite aqueous solution into a reaction kettle, keeping the temperature of the materials in the reaction kettle between 80 ℃ and 100 ℃ for 1h, cooling, adding 0.63g of composite bactericide (the composite bactericide comprises EDTA, sodium benzoate, sodium metabisulfite and sodium nitrate, and the mass ratio of the components is 2.
Example 3
Step 1: adding 300g of 60wt% DMDAAC aqueous solution into a reaction kettle, adding 18g of N-allyl morpholine, adding 0.144g of ethylene diamine tetraacetic acid disodium and 0.144g of sodium benzoate, stirring to completely dissolve, adding sodium hydroxide or hydrochloric acid to adjust the pH value to 6.0, heating the temperature of the reaction kettle materials to 90 ℃, introducing nitrogen from the bottom of the reaction kettle for 30min, wherein the nitrogen flow rate is 60m 3 /h。
Step 2: 36g of 4 wt% potassium persulfate aqueous solution and 240g of 50wt% acrylamide aqueous solution are respectively dropwise added into the reaction kettle at a certain flow rate, and the dropwise addition of the initiator is controlled within 5min after the functional monomer and the acrylamide aqueous solution is finished. The temperature of the materials in the reaction kettle is controlled to be 90-100 ℃ in the whole process. And after the addition of the potassium persulfate aqueous solution is finished, keeping the temperature of the materials in the reaction kettle at 90-100 ℃ for 1h.
And step 3: adding 15.43g of 35wt% sodium bisulfite aqueous solution into a reaction kettle, keeping the temperature of the materials in the reaction kettle between 80 ℃ and 100 ℃ for 1h, cooling, adding 0.9g of a composite bactericide (the composite bactericide comprises EDTA, sodium benzoate, sodium metabisulfite and sodium nitrate, and the mass ratio of the components is 2.
Comparative example 1
Step 1: adding 300g of 60wt% DMDAAC aqueous solution into a reaction kettle, adding 0.054g of ethylene diamine tetraacetic acid, adding 0.054g of sodium benzoate, stirring to completely dissolve, adding sodium hydroxide or hydrochloric acid to adjust the pH value to 6.2, heating the temperature of the materials in the reaction kettle to 90 ℃, introducing nitrogen from the bottom of the reaction kettle for 30min, wherein the nitrogen flow rate is 60m 3 /h。
Step 2: 36g of 1 wt% strength potassium persulfate aqueous solution and 360g of 50wt% strength acrylamide aqueous solution are respectively dripped into the reaction kettle at a certain flow rate, and the dripping of the initiator is controlled within 5min after the functional monomer and the acrylamide aqueous solution is finished. The temperature of the materials in the reaction kettle is controlled to be 90-100 ℃ in the whole process. And after the addition of the potassium persulfate aqueous solution is finished, keeping the temperature of the materials in the reaction kettle at 90-100 ℃ for 1h.
And 3, step 3: adding 5.14g of 35wt% sodium bisulfite aqueous solution into a reaction kettle, keeping the temperature of the materials in the reaction kettle between 80 ℃ and 100 ℃ for 1h, cooling, adding 0.36g of a composite bactericide (the composite bactericide comprises EDTA, sodium benzoate, sodium metabisulfite and sodium nitrate, and the mass ratio of the components is 2.
Comparative example 2
Step 1: adding 300g of 60wt% DMDAAC aqueous solution into a reaction kettle, adding 9g of N-allyl morpholine, adding 0.054g of ethylene diamine tetraacetic acid disodium and 0.054g of sodium benzoate, stirring until the solution is completely dissolved, adding sodium hydroxide or hydrochloric acid to adjust the pH value to 6.2, and reactingHeating the kettle material to 90 ℃, and introducing nitrogen for 30min from the bottom of the reaction kettle, wherein the nitrogen flow rate is 60m 3 /h。
Step 2: 36g of 1 wt% potassium persulfate aqueous solution and 360g of 50wt% acrylamide aqueous solution are respectively dripped into the reaction kettle at a certain flow rate, and the dripping is finished within 5min after the initiator is controlled to be the functional monomer and the acrylamide aqueous solution. The temperature of the materials in the reaction kettle is controlled to be 90-100 ℃ in the whole process. And after the addition of the potassium persulfate aqueous solution is finished, keeping the temperature of the materials in the reaction kettle at 90-100 ℃ for 1h.
And 3, step 3: 5.14g of 35wt% sodium bisulfite aqueous solution is added into a reaction kettle, the temperature of the materials in the reaction kettle is kept between 80 ℃ and 100 ℃ for 1h, and the liquid organic sludge dehydrating agent B2 is obtained after cooling and uniform stirring.
Detection example 1
The products obtained in the examples and comparative examples were subjected to physical and chemical index tests. (wherein, the method for testing the intrinsic viscosity refers to national standard GB/T33085-2016) and the specific test data is shown in the table:
discussion of the related Art
From the above table, it can be seen that the intrinsic viscosity of the products obtained in examples 1 to 3 is almost the same as that of the products obtained in comparative examples 1 to 2, but the products obtained in examples 1 to 3 are in a fluid state, no morpholine group is added in comparative example 1, and the product in comparative example 1 is in a gel state, which indicates that the addition of a morpholine-related structural monomer is beneficial to the reduction of the viscosity of the product.
Detection example 2
The following are the application experiments and results of sludge dewatering: the products obtained in examples 1 to 3 and comparative examples 1 to 2 were prepared into a sludge-dewatering agent solution of 2 g/l, 200ml of sludge was taken and added to 2ml of the previously prepared sludge-dewatering agent solution, and after uniform mixing, the mixture was added to a plate and frame filter press. Setting parameters, pressure 0.4Mpa, time 20min; the pressure is 0.8Mpa, and the time is 10min; the pressure is 2.0Mpa, the time is 20min, and the filter-pressed mud cake and the filtrate are taken out for testing; the turbidity of filtrate is measured by a turbidity meter (the equipment model is 2100N), the water content of filter cake is measured by a water analyzer (the equipment model is HE 53/02), and the specific resistance of sludge is measured by a specific resistance measuring instrument (the equipment model is ROCKER 300).
Note: the sludge comes from Chi Deni concentrated in a sewage treatment station of the factory, the water content is 98.56 percent, and the dried ash is black and yellow.
See the following table for specific experimental data:
discussion of the preferred embodiments
From the above application experiment results of sludge dewatering, it can be seen that the product of examples 1 to 3 is superior to ferric salt and cationic polyacrylamide in the water content of sludge cake, the turbidity of filtrate and the specific resistance of sludge, and the sludge dewatering performance is reduced to some extent without adding a functional monomer for comparative example 1, and the effect of the examples is not achieved without adding a composite bactericide for comparative example 2, which indicates that the addition of the functional monomer and the composite bactericide plays a synergistic role, so that the synthesized sludge dewatering agent has more excellent dewatering performance.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
Claims (6)
1. A method for preparing a liquid organic sludge dehydrating agent, which is characterized by comprising:
step 1, adding an aqueous solution of a cationic monomer into a reaction kettle, adding a functional structural monomer N-allyl morpholine, adding a metal ion chelating agent, adding a chain transfer agent, stirring to completely dissolve, adjusting the pH value to 5-7, heating the temperature of the reaction kettle material to 70-90 ℃, and introducing nitrogen into the reaction kettle;
step 2, respectively dripping an initiator aqueous solution and an acrylamide aqueous solution into the reaction kettle at a preset flow rate for 1-3h, and controlling the dripping of the initiator to be finished within 5-10min after the acrylamide aqueous solution; controlling the temperature of the materials in the reaction kettle to be 80-95 ℃ in the whole process; after the initiator is added, keeping the temperature of the materials in the reaction kettle at 80-90 ℃ and continuing to react for 0.5-2h;
step 3, adding a sodium bisulfite aqueous solution into the reaction kettle, and keeping the temperature of the materials in the reaction kettle between 80 and 100 ℃ to continue the reaction for 0.5 to 2 hours; cooling, namely adding the composite bactericide into the reaction kettle when the temperature of the reaction kettle is reduced to 30-50 ℃, and uniformly stirring to obtain a liquid organic sludge dehydrating agent;
the compound bactericide comprises EDTA, sodium benzoate, sodium metabisulfite and sodium nitrate; and the mass ratio of each component is 2:1:1:2;
the cationic monomer is one or more of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride, methacryloyloxyethyl dimethyl benzyl ammonium chloride, acryloylpropyltrimethyl ammonium chloride and dimethyl diallyl ammonium chloride;
the mass ratio of the cationic monomer to the acrylamide on a dry basis is 1-1.5; the dosage of the functional structural monomer is 5-10% of the mass of the dry-based cationic monomer.
2. The method for preparing a liquid organic sludge dehydrating agent according to claim 1, wherein the metal ion chelating agent is one or a mixture of sodium citrate, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate, sodium gluconate, and sodium tripolyphosphate.
3. The method for preparing a liquid organic sludge dehydrating agent according to claim 1, wherein the chain transfer agent is one or a mixture of sodium benzoate, sodium hypophosphite, sodium formate, sodium acetate and n-butanol.
4. The method for preparing a liquid organic sludge dehydrating agent according to claim 1, wherein the initiator is one or a mixture of potassium persulfate, sodium persulfate and ammonium persulfate.
5. The method for preparing a liquid organic sludge dehydrating agent according to claim 1, wherein the amount of the metal ion chelating agent is 0.03 to 0.08% by mass of the dry-based cationic monomer; the dosage of the chain transfer agent is 0.03-0.08% of the mass of the dry-based cationic monomer; the dosage of the initiator is 0.2 to 0.8 percent of the mass of the dry-based cationic monomer; the dry basis amount of sodium bisulfite in the sodium bisulfite aqueous solution is 1 to 3 percent of the mass of the dry basis cationic monomer; the dosage of the composite bactericide is 0.2-0.5% of the mass of the dry-based cationic monomer.
6. A liquid organic sludge-dewatering agent obtained by the method for producing a liquid organic sludge-dewatering agent according to any one of claims 1 to 5.
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