CN117228800A - Circulating water treatment agent and preparation method thereof - Google Patents
Circulating water treatment agent and preparation method thereof Download PDFInfo
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- CN117228800A CN117228800A CN202311272859.3A CN202311272859A CN117228800A CN 117228800 A CN117228800 A CN 117228800A CN 202311272859 A CN202311272859 A CN 202311272859A CN 117228800 A CN117228800 A CN 117228800A
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- ammonium salt
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Landscapes
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
Abstract
The invention discloses a circulating water treatment agent and a preparation method thereof, which belong to the technical field of water treatment, wherein the circulating water treatment agent comprises the following raw materials in parts by weight: 25-35 parts of white radish stem and leaf extract, 15-20 parts of sweet potato extract, 10-20 parts of licorice extract, 15-30 parts of poly serine modified polyepoxysuccinic acid and 4-20 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, in the sepiolite fiber/chitosan quaternary ammonium salt complex, 1-5 parts of sepiolite fiber and 3-15 parts of chitosan quaternary ammonium salt are wrapped in the holes of the sepiolite fiber. The water treatment agent prepared finally is mainly derived from natural products, does not cause secondary pollution to the environment, and the components are mutually matched, so that the water treatment agent has good corrosion inhibition effect, scale inhibition effect and sterilization effect, is a water treatment agent with low cost, high scale inhibition and corrosion inhibition efficiency and environment-friendly property, and has good application prospect in water treatment of a cooling water circulation system.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a circulating water treatment agent and a preparation method thereof.
Background
Water is an extremely valuable material resource for human survival and in the field of industrial and agricultural production. With the rapid development of industry and agriculture, the industrial water consumption is increasingly increased, and more than 80% of the water consumption is occupied, so that the circulating water becomes an important means for saving water resources, wherein the industrial circulating cooling water accounts for 70% -90% of the total industrial water. The repeated use of the cooling water can increase the scale ion content of the circulating water, gradually worsen the water quality, scale on the heat exchange equipment and influence the normal use of the equipment. The water treatment agent can prevent the circulating water from scaling, corrosion and biological slime caused by high concentration multiple and long-period running, thus causing a series of problems of pipeline blockage, corrosion leakage, greatly reduced heat transfer efficiency and the like.
Currently, phosphorus scale and corrosion inhibitors and organic scale and corrosion inhibitors are commonly used in countries around the world, and the phosphorus scale and corrosion inhibitors generally contain high electronegativity atoms (such as nitrogen, oxygen, sulfur and phosphorus), such as arsenate, phosphate, chromate and the like; organic scale and corrosion inhibitors are mostly organic heterocyclic compounds containing unsaturated bonds or large conjugated systems, such as azoles, schiff bases, pyridine and the like. The scale and corrosion inhibitor is easy to synthesize and apply, has high scale and corrosion inhibition efficiency under lower concentration, but has high cost and toxicity, can cause secondary pollution to the environment, for example, the phosphate corrosion inhibitor can also cause eutrophication of water body, and limits the development and application prospect. Therefore, with the enhancement of people's environmental awareness, it is necessary to study a water treatment agent which has low cost, high scale and corrosion inhibition efficiency and is friendly to the environment.
The plant extract has been proved to avoid corrosion of metal materials, and compared with the traditional synthetic water treatment agent, the plant extract has the advantages of convenient extraction, low cost, environmental friendliness and wide development prospect.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a water treatment agent which has low cost, high scale and corrosion inhibition efficiency and is environment-friendly.
The second object of the present invention is to provide a method for producing a circulating water treatment agent, which is simple in steps and can industrially produce a circulating water treatment agent.
The invention adopts the following technical scheme for realizing one of the purposes:
the circulating water treatment agent is characterized by comprising the following raw materials in parts by weight: 25-35 parts of white radish stem and leaf extract, 15-20 parts of sweet potato extract, 10-20 parts of licorice extract, 15-30 parts of poly serine modified polyepoxysuccinic acid and 4-20 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, in the sepiolite fiber/chitosan quaternary ammonium salt compound, 1-5 parts of sepiolite fiber and 3-15 parts of chitosan quaternary ammonium salt are wrapped in the holes of the sepiolite fiber.
Further, the raw materials according to the weight parts are preferably as follows: 30 parts of white radish stem and leaf extract, 20 parts of sweet potato extract, 15 parts of licorice extract, 25 parts of poly serine modified polyepoxysuccinic acid and 9 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; in the sepiolite fiber/chitosan quaternary ammonium salt complex, 3 parts of sepiolite fiber and 6 parts of chitosan quaternary ammonium salt are wrapped in the holes of the sepiolite fiber.
Further, the sepiolite fiber/chitosan quaternary ammonium salt composite comprises the following sepiolite fibers and chitosan quaternary ammonium salt in a weight ratio of 3:1.
furthermore, in the sepiolite fiber/chitosan quaternary ammonium salt complex, the pore canal of the sepiolite fiber is columnar, and the fiber arrangement is more regular.
The second technical scheme adopted by the invention for realizing the second purpose is as follows:
the invention provides a preparation method of a circulating water treatment agent, which comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain the white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain the raw sweet potato extract;
s3, dissolving polyepoxysuccinic acid in water, adding polyserine, heating to 90 ℃, regulating the rotating speed to react, and then drying in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain the sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain the chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
In the invention, the white radish stem and leaf extract is a mixed scale and corrosion inhibitor mainly used as a cathode, which can slow down and limit the reaction of hydrogen precipitation in a cathode corrosion medium and slow down and limit the reaction of anode metal dissolution. The white radish stem and leaf extract mainly contains the ascorbic acid, folic acid, catechin, o-coumaric acid and 4-methylthio-3-butenyl thioglycoside, and the adsorption on the surface of the carbon steel accords with the Langmuir adsorption model and the like, and the corrosion inhibition mechanism is that the extract is adsorbed on the surface of the carbon steel to form a thin and compact protective film, so that the corrosion of corrosive mediums is prevented. The molecular ascorbic acid, nicotinic acid and chlorogenic acid in the sweet potato extract contain more N, O heteroatoms, aromatic rings and multiple bonds, and the lone pair electrons and conjugated pi bonds of the molecular ascorbic acid, nicotinic acid and chlorogenic acid can coordinate with iron-air orbitals, so that the adsorption capacity is stronger. The licorice extract contains glycyrrhizin, 18 beta-glycyrrhetinic acid, licochalcone-A and other component molecules, and can form a layer of protecting film on the surface of steel, and the protecting film can increase the contact angle of water drops on the surface of steel and enhance the hydrophobicity. The white radish stem and leaf extract, the sweet potato extract and the licorice extract can synergistically increase the corrosion inhibition effect, a layer of thicker, compact and uniform corrosion inhibition film can be formed in a water circulation system by using the white radish stem and leaf extract and the sweet potato extract, the electric charge transfer resistance can be increased, the anode reaction is inhibited, the corrosion reaction rate is greatly reduced, the hydrophobicity of the metal surface of the cooling water circulation system is enhanced by using the licorice extract, the contact with water drops of the cooling water circulation system is reduced, and the corrosion of corrosive mediums is fundamentally prevented.
The polyepoxysuccinic acid has no toxicity, high scale inhibiting activity, excellent biodegradability and alkali resistance, and may be used in water system with high alkalinity and high hardness to match Ca in water 2+ 、Mg 2+ The equimetal cations are chelated to form stable chelate, so that Ca is reduced 2 + 、Mg 2+ Isobustion cations and CO 3 2- The frequency of collision bonding of the scale forming anions is equal. According to the invention, the polyepoxysuccinic acid and the polyserine are subjected to graft copolymerization, and compared with single polyepoxysuccinic acid, the polyepoxysuccinic acid is added with negative groups such as hydroxyl groups, carboxyl groups and amide groups, so that the chelating capacity of the polyepoxysuccinic acid to scale forming cations is improved, the solubility of metal cations in water is further increased, in addition, the negative groups are increased, the capability of absorbing scale microcrystals by chains is enhanced, the distortion effect of the scale microcrystals is increased, the scale growth is enlarged, and the better scale inhibition and dispersion effects are achieved.
The chitosan quaternary ammonium salt is a chitosan derivative, has biocompatibility, has the property of amphoteric polyelectrolyte, has more active groups such as hydroxyl, amino, carboxyl and the like, has high water solubility and high charge density, and has the effects of sterilizing and killing algae; sepiolite fibers have good adsorption capacity. According to the invention, the chitosan quaternary ammonium salt and the sepiolite fiber are compounded to prepare the chitosan quaternary ammonium salt/sepiolite fiber complex, wherein the chitosan quaternary ammonium salt is wrapped on the sepiolite fiber in the complex, the porous property and the huge surface area of the sepiolite fiber can enable the active group of the chitosan quaternary ammonium salt to be better in dispersibility and easier to contact microorganisms in circulating cooling water, the chitosan quaternary ammonium salt and the sepiolite fiber complex are synergistic, the sterilization and algae killing effects are improved, and the chitosan quaternary ammonium salt/sepiolite fiber complex can absorb bacteria and algae and kill bacteria and play a role of stripping biological mud precipitation so as to control dirt accumulated in a circulating cooling water system and bacteria growing under dirt.
The sterilizing algicide polysaccharide quaternary ammonium salt/sepiolite fiber complex in a circulating cooling water system can strip accumulated dirt and biological mud precipitate during sterilizing and algae killing, and provides friendly environment for corrosion inhibitor white radish stem and leaf extract, sweet potato extract and licorice extract, so that a layer of thicker, compact and uniform corrosion inhibition film can be formed rapidly, metal corrosion is prevented, the tryptophan modified polyepoxysuccinic acid plays the role of a scale inhibitor to chelate with metal ions in water, and the water treatment agent plays a synergistic effect from three aspects of scale inhibition, corrosion inhibition, sterilization and algae killing, and plays the efficacy of each medicament to the maximum extent.
Compared with the prior art, the invention has the beneficial effects that:
(1) The water treatment agent provided by the invention does not contain phosphorus and is environment-friendly;
(2) Compared with the traditional synthetic water treatment agent, the water treatment agent provided by the invention mainly originates from natural products, has convenient extraction of natural extracts, low cost, biodegradability and reproducibility,
(3) The components of the water treatment agent provided by the invention are mutually cooperated, so that the water treatment agent has good corrosion inhibition effect, scale inhibition effect and sterilization effect.
(4) The water treatment agent provided by the invention is a small amount of CaCO 3 And CaPO (CaPO) 4 The static scale inhibition rate can reach more than 99.7% and more than 95.7%, so that the corrosion rate of the carbon steel is lower than 0.0125mm/a, the corrosion rates of red copper and stainless steel are lower than 0.0023mm/a, and the sterilization rate reaches 97.38%.
Detailed Description
The present invention will be further described with reference to specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
Example 1
The circulating water treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 25 parts of white radish stem and leaf extract, 25 parts of sweet potato extract, 10 parts of licorice extract, 35 parts of poly serine modified polyepoxysuccinic acid and 20 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, the sepiolite fiber is 5 parts and the chitosan quaternary ammonium salt is 15 parts.
The preparation method of the circulating water treatment agent provided by the embodiment specifically comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain a raw sweet potato extract;
s3, according to the method, the polyepoxysuccinic acid is dissolved in water, then the polyserine is added, the temperature is raised to 90 ℃, the rotating speed is adjusted to react, and then the polyepoxysuccinic acid is dried in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
Example 2
The circulating water treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 35 parts of white radish stem and leaf extract, 15 parts of sweet potato extract, 20 parts of licorice extract, 15 parts of poly serine modified polyepoxysuccinic acid, and 4 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, sepiolite fiber 1 part and chitosan quaternary ammonium salt 3 parts.
The preparation method of the circulating water treatment agent provided by the embodiment specifically comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain a raw sweet potato extract;
s3, according to the method, the polyepoxysuccinic acid is dissolved in water, then the polyserine is added, the temperature is raised to 90 ℃, the rotating speed is adjusted to react, and then the polyepoxysuccinic acid is dried in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
Example 3
The circulating water treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 30 parts of white radish stem and leaf extract, 20 parts of sweet potato extract, 15 parts of licorice extract, 25 parts of poly serine modified polyepoxysuccinic acid and 12 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, sepiolite fiber 3 parts and chitosan quaternary ammonium salt 9 parts.
The preparation method of the circulating water treatment agent provided by the embodiment specifically comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain a raw sweet potato extract;
s3, according to the method, the polyepoxysuccinic acid is dissolved in water, then the polyserine is added, the temperature is raised to 90 ℃, the rotating speed is adjusted to react, and then the polyepoxysuccinic acid is dried in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, and fixing after separationDrying the body material at 75 ℃, and crushing to obtain chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
Example 4
The circulating water treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 27 parts of white radish stem and leaf extract, 23 parts of sweet potato extract, 18 parts of licorice extract, 30 parts of polyserine modified polyepoxysuccinic acid and 8 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, sepiolite fiber 2 parts and chitosan quaternary ammonium salt 6 parts.
The preparation method of the circulating water treatment agent provided by the embodiment specifically comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain a raw sweet potato extract;
s3, according to the method, the polyepoxysuccinic acid is dissolved in water, then the polyserine is added, the temperature is raised to 90 ℃, the rotating speed is adjusted to react, and then the polyepoxysuccinic acid is dried in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, and then adding the sea with the formula amountAfter stirring for 2 hours in the mineral wool suspension, the pH value is adjusted to 9.0 by 0.5mol/L sodium hydroxide solution, and a centrifuge is used for 10000 timesrpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
Example 5
The circulating water treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 32 parts of white radish stem and leaf extract, 28 parts of sweet potato extract, 12 parts of licorice extract, 20 parts of polyserine modified polyepoxysuccinic acid, and 16 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, the sepiolite fiber is 4 parts, the chitosan quaternary ammonium salt is 12 parts.
The preparation method of the circulating water treatment agent provided by the embodiment specifically comprises the following steps:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain a raw sweet potato extract;
s3, according to the method, the polyepoxysuccinic acid is dissolved in water, then the polyserine is added, the temperature is raised to 90 ℃, the rotating speed is adjusted to react, and then the polyepoxysuccinic acid is dried in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
Comparative example 1
The difference from example 1 is that the white radish stem and leaf extract is not added.
Comparative example 2
The difference from example 1 is that sweet potato extract was not added.
Comparative example 3
The difference from example 1 is that no licorice extract was added.
Comparative example 4
The difference from example 1 is that the polyserine was not modified for polyepoxysuccinic acid.
Comparative example 5
The difference from example 1 is that sepiolite fiber was not complexed with chitosan quaternary ammonium salt.
Experimental example
1 Experimental method
The dosage of the water treatment agent is 10mg/L, and the method for measuring the scale inhibition performance of the water treatment agent is a static scale inhibition method, and refers to a calcium carbonate deposition method (GB/T16632-2008) for measuring the scale inhibition performance of the water treatment agent and a calcium phosphate deposition method (GB/T22626-2008) for measuring the scale inhibition performance of the water treatment agent. Static scale inhibition performance test conditions of calcium carbonate: the calcium ion concentration was 250mg/L, the bicarbonate ion concentration was 250mg/L, and the experiment was performed at 80℃for 10 hours. Static scale inhibition performance experimental conditions of calcium phosphate: the laboratory water is prepared water, wherein the calcium ion concentration is 250mg/L, the phosphate ion concentration is 5mg/L, the prepared water is not concentrated, and the experimental temperature is 80 ℃ and the time is 10 hours;
the method for measuring the corrosion inhibition performance of the water treatment agent is a rotary hanging piece method, and refers to a 'water treatment agent corrosion inhibition performance measurement-rotary hanging piece method' (GB/T18175-2000), test pieces are carbon steel hanging pieces, red copper hanging pieces and stainless steel hanging pieces, the test temperature is 60 ℃, the test piece rotating speed is 75 revolutions per minute, the rotating linear speed is 0.35 m/s, and the test time is 72 hours;
the sterilization rate of the water treatment agent is tested by adopting a heterotrophic bacteria plate counting method.
2 determination of Water quality basic Performance index
The quality measurement experiment of the circulating cooling water or the supplementing water mainly comprises the pH value, the total hardness (total calcium and magnesium turbidity), the total alkalinity, the calcium content, the chlorine content, the iron content, the potassium sulfide content and the like, and the methods and the index values referred by various performance tests are shown in the table 1.
TABLE 1 analysis of Water quality of circulating Cooling Water or make-up Water
3 results of experiments
TABLE 2 comparison of the effects of the water treatment agents of examples and comparative examples
Experiments in the above examples 1-5 show that the water treatment agent of the invention can inhibit scale and corrosionAnd sterilizing effect, caCO when the amount is 10m/L 3 The scale inhibition rate reaches more than 99.7 percent, caPO 4 The scale inhibition rate reaches more than 97.0%, the corrosion rate of carbon steel is lower than 0.0125mm/a, the corrosion rates of red copper and stainless steel are lower than 0.0023mm/a, and the sterilization rate reaches more than 97.38%.
As is clear from the comparison of the example 1 and the comparative examples 1-3, the white radish stem and leaf extract, the sweet potato extract and the licorice extract have good synergistic corrosion inhibition effect; as can be seen from a comparison of example 1 with comparative example 4, comparative example 4 did not modify the CaCO of polyserine to polycyclosuccinic acid 3 The scale inhibition rate is 83.31%, caPO 4 The scale inhibition was 83.21%, and after the modification of polyepoxysuccinic acid with polyserine in example 1, caCO was used 3 The scale inhibition rate is 99.82%, caPO 4 The scale inhibition rate is 97.32%, which shows that the scale inhibition effect of the poly-serine modified polyepoxysuccinic acid can increase the scale inhibition effect of the polyepoxysuccinic acid; as can be seen from the comparison between example 1 and comparative example 5, the sterilization rate of comparative example 5 in which sepiolite fibers and chitosan quaternary ammonium salt are not compounded is 82.50%, and the sterilization rate of example 1 in which sepiolite fibers and chitosan quaternary ammonium salt are compounded is 97.38%, indicating that sepiolite fibers can enhance the sterilization effect of chitosan quaternary ammonium salt.
In conclusion, the corrosion inhibition efficiency of the circulating water treatment agent is more than 98.9% when the corrosion rate is far less than 0.075mm/a required by the national standard. At the same time, caCO thereof 3 And CaPO (CaPO) 4 The static scale inhibition rate is respectively more than 99.7 percent and more than 95.7 percent, and the sterilization efficiency is about 97 percent.
Compared with the prior art, the water treatment agent provided by the invention is nontoxic, does not contain phosphorus, and is environment-friendly; the raw material sources are wide, and the cost is low; in addition, the components of the water treatment agent provided by the invention are mutually cooperated, so that good corrosion inhibition effect, scale inhibition effect and sterilization effect are shown, and the water treatment agent provided by the invention has obvious corrosion inhibition performance, scale inhibition performance and sterilization performance and is environment-friendly.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.
Claims (5)
1. The circulating water treatment agent is characterized by comprising the following raw materials in parts by weight: 25-35 parts of white radish stem and leaf extract, 15-20 parts of sweet potato extract, 10-20 parts of licorice extract, 15-30 parts of poly serine modified polyepoxysuccinic acid and 4-20 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; wherein, in the sepiolite fiber/chitosan quaternary ammonium salt compound, 1-5 parts of sepiolite fiber and 3-15 parts of chitosan quaternary ammonium salt are wrapped in the holes of the sepiolite fiber.
2. The circulating water treatment agent as claimed in claim 1, wherein the raw materials in parts by weight are preferably: 30 parts of white radish stem and leaf extract, 20 parts of sweet potato extract, 15 parts of licorice extract, 25 parts of poly serine modified polyepoxysuccinic acid and 9 parts of sepiolite fiber/chitosan quaternary ammonium salt complex; in the sepiolite fiber/chitosan quaternary ammonium salt complex, 3 parts of sepiolite fiber and 6 parts of chitosan quaternary ammonium salt are wrapped in the holes of the sepiolite fiber.
3. A circulating water treatment agent as claimed in claim 1 or 2, wherein the sepiolite fibres / The weight ratio of sepiolite fiber and chitosan quaternary ammonium salt in the chitosan quaternary ammonium salt complex is 3:1.
4. the circulating water treatment agent as claimed in claim 1 or 2, wherein in the sepiolite fiber/chitosan quaternary ammonium salt complex, the sepiolite fiber has no impurity in the pore canal, the pore canal is columnar, and the fiber arrangement is regular.
5. A method for preparing the circulating water treatment agent according to claim 1 or 2, comprising the steps of:
s1, drying and crushing white radish stems and leaves, adding 500mL of water, leaching for 48 hours at room temperature, performing ultrasonic treatment at 60 ℃ for 40 minutes, cooling to room temperature, filtering, concentrating filtrate by using a rotary evaporator, and drying at 60 ℃ to obtain the white radish stem and leaf extract;
s2, peeling and crushing the sweet potatoes, adding water, carrying out ultrasonic treatment for 30min, heating at 60 ℃ for 5h, cooling to room temperature, filtering to remove solid residues, standing filtrate for 48h, removing starch, and concentrating the filtrate in a rotary evaporator to obtain the raw sweet potato extract;
s3, dissolving polyepoxysuccinic acid in water, adding polyserine, heating to 90 ℃, regulating the rotating speed to react, and then drying in a dryer at 45 ℃ to obtain the polyepoxysuccinic acid modified by the polyserine;
s4, adding natural sepiolite fibers into hydrochloric acid with the concentration of 0.8mol/L according to the solid-to-liquid ratio of 1:10, carrying out water bath at 80 ℃ for 8 hours, carrying out centrifugal separation, washing the solid with water for 3 times, putting the solid into an oven, respectively heating at 250 ℃ for 2 hours, cooling to room temperature, and crushing to 80 meshes to obtain the sepiolite fibers;
s5, adding the chitosan quaternary ammonium salt with the formula amount into acetic acid solution with the mass concentration of 1% for uniform stirring, adding the chitosan quaternary ammonium salt with the formula amount into sepiolite fiber suspension for stirring for 2 hours, adjusting the pH value to 9.0 by using sodium hydroxide solution with the concentration of 0.5mol/L, and using a centrifuge for stirring at 10000rpmAfter centrifugation for 15min at the rotating speed, separating, drying the separated solid substance at 75 ℃, and crushing to obtain the chitosan quaternary ammonium salt/sepiolite fiber complex;
s6, uniformly mixing the white radish stem and leaf extract, the sweet potato extract, the licorice extract, the polyserine modified polyepoxysuccinic acid and the chitosan quaternary ammonium salt/modified stone fiber complex according to the formula amount to obtain the circulating water treatment agent.
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