CN111762900B - Phosphorus-free composite water treatment agent and application thereof - Google Patents
Phosphorus-free composite water treatment agent and application thereof Download PDFInfo
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- CN111762900B CN111762900B CN202010654807.2A CN202010654807A CN111762900B CN 111762900 B CN111762900 B CN 111762900B CN 202010654807 A CN202010654807 A CN 202010654807A CN 111762900 B CN111762900 B CN 111762900B
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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
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen
- C02F5/125—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen combined with inorganic substances
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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
- C02F2303/00—Specific treatment goals
- C02F2303/08—Corrosion inhibition
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Abstract
The invention discloses a phosphorus-free composite water treatment agent and application thereof; relates to the technical field of water treatment, and is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water in water bath at the temperature; the stirring reaction is treated by ultrasonic waves; the water treated by the water treatment agent prepared by the method does not contain phosphorus elements, so that the threat of water eutrophication is greatly reduced, the water quality is greatly improved, and the water can be better recycled.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a phosphorus-free composite water treatment agent and application thereof.
Background
With the increasing severity of environmental problems, people's environmental awareness is strengthened more and more, the traditional water treatment agent generally contains phosphorus element and can promote the water treatment effect, but the water quality treated by the phosphorus-containing water treatment agent contains phosphorus element with higher concentration, which causes water eutrophication.
According to the requirements of energy conservation and emission reduction, more and more circulating water farms save fresh water by increasing the concentration multiple of circulating water and using a large amount of regenerated water as the replenishing water of the circulating water, thereby causing some problems. The turbidity of the circulating water is increased continuously while the concentration multiple is improved, the quality of the regenerated water is poorer than that of fresh water, and the turbidity of the circulating water after concentration is higher. The turbidity of the circulating water is increased, suspended substances in the water are easy to deposit in the circulating water system to form dirt, and colloidal substances can form cohesive dirt, promote the dirt deposition and cause local corrosion. At present, the water quality stability of circulating water is mainly controlled by respectively adding a scale inhibitor and a corrosion inhibitor in the running process of a circulating cooling water system, however, the existing corrosion inhibitor has a common treatment effect, and further improvement on the performance of the existing corrosion inhibitor is needed to improve the application range of the corrosion inhibitor. In addition, the pollution of water by phosphorus-containing compounds and the resulting eutrophication of water have led to a growing recognition of the importance of controlling the discharge of phosphorus-containing compounds. A lot of rivers and lakes around the world cause uncontrolled growth of aquatic plants due to discharge of a large amount of phosphorus, dissolved oxygen in water is exhausted, and finally water quality is deteriorated and aquatic animals and plants are extinct. With the increase of awareness of environmental protection and further strictness of environmental regulations, many places in China have come to limit the use of phosphorus-containing products in recent years, so that the development of low-phosphorus and phosphorus-free water treatment agents has become a research hotspot.
Disclosure of Invention
The invention aims to provide a phosphorus-free composite water treatment agent and application thereof, so as to solve the defects in the prior art.
The technical scheme adopted by the invention is as follows:
a non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath;
the stirring reaction is treated by ultrasonic waves;
the stirring reaction is treated by ultrasonic waves;
the preparation method of the rare earth modified diatomite comprises the following steps:
(1) heating diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1-1.5 hours, then taking out, and naturally cooling;
the vacuum degree is 0.02 MPa;
the particle size of the diatomite is 30 μm;
(2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid;
the acid solution is a citric acid solution;
the citric acid solution accounts for 5% by mass;
the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL;
the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution;
(3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion liquid into the diatomite dispersion liquid, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion liquid;
the rare earth is lanthanum chloride;
the mass fraction of lanthanum chloride is 0.002-0.003%;
the drying temperature is 200 ℃.
As a further technical scheme: the acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 15-18: 12-16:8-10:80-86, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 40-60 mg/L.
As a further technical scheme, the method is characterized in that: the acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer.
As a further technical scheme, the method is characterized in that: the sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate.
As a further technical scheme: the temperature of the water bath is 90-92 ℃;
as a further technical scheme: the ultrasonic treatment frequency is 35kHz, and the power is 500W.
An application of a phosphorus-free composite water treatment agent in the field of water treatment.
Has the advantages that:
the invention provides a phosphorus-free composite water treatment agent and application thereof, and water treated by the water treatment agent prepared by the method does not contain phosphorus elements, so that the threat of water eutrophication is greatly reduced, the water quality is greatly improved, and the phosphorus-free composite water treatment agent can be better recycled;
the phosphorus-free composite water treatment agent prepared by the invention has an excellent corrosion inhibition function, can greatly reduce the corrosion effect of treated water, and greatly improves the quality of the treated water;
according to the invention, a polarization test shows that the polarization curve is obviously shifted forwards after the tetradecyl monoester sulfonate sulfosuccinate is added, and the larger the forward shift offset of the self-corrosion potential is along with the increase of the concentration of the tetradecyl monoester sulfonate sulfosuccinate, the addition of the tetradecyl monoester sulfonate sulfosuccinate has the function of greatly improving the corrosion inhibition performance;
according to the invention, through the synergistic effect of the components, a thin adsorption film can be formed on the surface of an corroded object, so that the contact with a corrosive medium can be isolated to a certain extent.
Drawings
Fig. 1 is a polarization graph.
FIG. 2 is a drawing of rare earth-modified diatomaceous earth xrd.
FIG. 3 is a graph of a blank sample after carbon steel has been corroded.
FIG. 4 shows the etched carbon steel sheet of example 6.
Detailed Description
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath;
the stirring reaction is treated by ultrasonic waves;
the stirring reaction is treated by ultrasonic waves;
the preparation method of the rare earth modified diatomite comprises the following steps:
(1) heating diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1-1.5 hours, then taking out, and naturally cooling;
the vacuum degree is 0.02 MPa;
the particle size of the diatomite is 30 μm;
(2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid;
the acid solution is a citric acid solution;
the citric acid solution accounts for 5% by mass;
the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL;
the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution;
(3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion;
the rare earth is lanthanum chloride;
the mass fraction of lanthanum chloride is 0.002-0.003%;
the drying temperature is 200 ℃.
As a further technical scheme: the acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 15-18: 12-16:8-10:80-86, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 40-60 mg/L.
As a further technical scheme, the method is characterized in that: the acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer.
As a further technical scheme, the method is characterized in that: the sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate.
As a further technical scheme: the temperature of the water bath is 90-92 ℃;
as a further technical scheme: the ultrasonic treatment frequency is 35kHz, and the power is 500W.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, 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.
Example 1
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the stirring reaction is treated by ultrasonic wave; the preparation method of the rare earth modified diatomite comprises the following steps:
(1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1 hour, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.002%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 25:12:8:80, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 40 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying until the weight is constant. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 90 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Example 2
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the preparation method of the rare earth modified diatomite comprises the following steps: (1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1.5 hours, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.003%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 29:16:10:86, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 45 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying until the weight is constant. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 92 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Example 3
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the preparation method of the rare earth modified diatomite comprises the following steps: (1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1.2 hours, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.0022%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 25:13:9:82, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 50 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying until the weight is constant. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 91 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Example 4
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the preparation method of the rare earth modified diatomite comprises the following steps: (1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1.5 hours, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.0024%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 26:15:9:83, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 55 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying to constant weight to obtain the rare earth modified diatomite. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 92 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Example 5
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the preparation method of the rare earth modified diatomite comprises the following steps: (1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1.5 hours, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.0028%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 28:13:9:82, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 60 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying until the weight is constant. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 90 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Example 6
A non-phosphorus composite water treatment agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic acid copolymer, sodium tartrate, rare earth modified diatomite and water at the temperature of water bath; the preparation method of the rare earth modified diatomite comprises the following steps: (1) heating the diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1 hour, then taking out, and naturally cooling; the vacuum degree is 0.02 MPa; the particle size of the diatomite is 30 μm; (2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid; the acid solution is a citric acid solution; the citric acid solution accounts for 5% by mass; the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL; the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution; (3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion; the rare earth is lanthanum chloride; the mass fraction of lanthanum chloride is 0.007%; the drying temperature is 200 ℃; the stirring reaction is treated by ultrasonic wave. The acrylic copolymer, the sodium tartrate, the rare earth modified diatomite and the water are mixed according to the weight ratio: 27:16:8:86, and the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate is 58 mg/L. The acrylic acid copolymer is an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer. The sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate. The preparation method of the sodium tetradecyl sulfosuccinate comprises the following steps: adding tetradecanol and maleic anhydride into a reaction kettle in sequence, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, then adding a catalyst and toluene, stirring at the rotating speed of 500r/min for 10min, then heating to 112 ℃, then continuing stirring for reaction for 8 hours, then detecting that the esterification rate reaches 50%, recrystallizing with methanol, and then drying to obtain an intermediate product; and sequentially adding the intermediate product, the rare earth modified diatomite and the propanol into a reaction kettle, heating to 85 ℃, keeping the temperature, stirring, reacting for 2 hours, and then carrying out rotary drying until the weight is constant. The molar ratio of the tetradecanol to the maleic anhydride is 1: 2. The catalyst is sodium acetate; the addition amount of the sodium acetate is 10 percent of the mass of the sodium maleate. The mixing mass ratio of the toluene to the maleic anhydride is 1: 1. The temperature of the water bath is 92 ℃; the ultrasonic treatment frequency is 35kHz, and the power is 500W.
Test of
Water quality parameter of test
TABLE 1
| Index (es) | Sample water |
| pH | 7.52 |
| Conductivity μ s/cm | 358 |
| Total alkalinity mg/L | 82 |
| Clmg/L | 65 |
| Total hardness mg/L | 135 |
The test method comprises the following steps:
soaking the carbon steel sheet in absolute ethyl alcohol for 10min, then wiping each sample by using not less than 50mL of reagent with filter paper, sucking the sample to dry, drying the sample in a drying device, weighing and recording;
the treatment tests were carried out with the treatment agents of examples and comparative examples, respectively;
adding the water treatment agent to the concentration, calculating the adding amount of the water treatment agent, adding the water treatment agent into a 1000mL beaker, accurately measuring the adding amount of the water treatment agent to 0.1mL, adding 1000mL of sample water, uniformly stirring, and drawing liquid level scale marks on the outer wall of the beaker;
when the temperature of the test solution reaches 40 +/-1 ℃, hanging the carbon steel sheet into a beaker, enabling the interval between the upper end of the carbon steel sheet and the liquid level to be more than 2cm and the interval between the lower end of the carbon steel sheet and the bottom of the beaker to be more than 3cm, starting a motor, enabling the carbon steel sheet to rotate at the rotating speed of 90r/min, and starting timing;
the beaker is in an open state, so that the test solution is naturally evaporated, pure water is added into the beaker every 4 hours during the test period, the liquid level is kept at the position of the graduation line again, and after 72 hours, the rotation is stopped, and the carbon steel sheet is taken out; scrubbing a carbon steel sheet by using a brush, then soaking the carbon steel sheet in an acid pickling solution for 30s, taking out, immediately washing the carbon steel sheet by using tap water, then soaking the carbon steel sheet in a sodium hydroxide solution for 30s, taking out, washing the carbon steel sheet by using tap water, wiping the carbon steel sheet by using filter paper to be dry, soaking the carbon steel sheet in absolute ethyl alcohol for 3min, taking out, placing the carbon steel sheet on clean filter paper, sucking the carbon steel sheet by using the filter paper, weighing the carbon steel sheet after constant weight for 4 hours in a dryer, and simultaneously performing an acid pickling blank test on the carbon steel sheet to correct acid pickling weight loss; corrosion rate A calculation
A＝87600(m-m0)/spt
m-carbon steel mass loss before test, g;
m 0-acid wash blank test mass loss, g;
surface area of s-carbon steel, cm2，20cm2；
Density of p-carbon steel, g/cm3，7.86g/cm3；
t-test time, h, 72 h;
calculating the slow release rate n:
n＝(A0-A1)/A0×100％
a0-carbon steel corrosion rate in blank test solution, mm/a;
a1-carbon steel corrosion rate in the test solution added with the treating agent, mm/a;
TABLE 2
Comparative example 1: only differs from example 1 in that no sulfosuccinic acid tetradecyl monoester sulfonate is added;
comparative example 2: only distinguished from example 1 by the absence of addition of acrylic copolymer;
as can be seen from Table 2, the water treatment agent prepared by the method has excellent corrosion inhibition function, can greatly reduce the corrosion effect of the treated water, and greatly improves the quality of the treated water.
As shown in fig. 1, the corrosion inhibition performance of the tetradecyl sulfosuccinate sulfonate is studied by a polarization curve test, wherein tetradecyl sulfosuccinate sulfonate with a mass concentration of 0-20,/4/60 mg/L is added into a test solution at room temperature, and after soaking for 30min, the polarization curve is measured, and the test result is shown in fig. 1;
TABLE 3
| Concentration mg/L | Sustained release rate/%) |
| 0 | / |
| 20 | 25.34 |
| 40 | 73.21 |
| 60 | 75.37 |
As shown in fig. 1, compared with a blank test polarization curve, the polarization curve after adding the sodium tetradecyl sulfosuccinate is obviously shifted positively, and the offset of positive shift of self-corrosion potential is larger along with the increase of the concentration of the sodium tetradecyl sulfosuccinate, which indicates that the addition of the sodium tetradecyl sulfosuccinate has a great function of improving corrosion inhibition performance;
as shown in Table 3, the corrosion inhibition effect is greatly improved with the increase of the concentration of the sulfosuccinic acid tetradecyl monoester sulfonate.
FIG. 2 is a drawing of rare earth-modified diatomaceous earth xrd.
Fig. 3 is a graph showing the appearance of a blank sample after carbon steel is corroded, fig. 4 is a graph showing the appearance of a carbon steel sheet in example 6 after the carbon steel sheet is corroded, and it can be seen from fig. 3 and fig. 4 that the blank sample has obvious corrosion on the surface of the carbon steel sheet, while the corrosion effect of sample water treated by the chemical in example 6 on the surface of the carbon steel sheet is greatly reduced, and it can be seen that the corrosion performance of the sample treated by the chemical in the invention is greatly reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.
Claims (4)
1. A non-phosphorus composite water treatment agent is characterized in that the agent is prepared by uniformly stirring and reacting tetradecyl sulfosuccinate sulfonate, acrylic copolymer, sodium tartrate, rare earth modified diatomite and water in water bath at a temperature;
the stirring reaction is treated by ultrasonic waves;
the preparation method of the rare earth modified diatomite comprises the following steps:
(1) heating diatomite to 400 ℃ under vacuum, then carrying out heat preservation treatment for 1-1.5 hours, then taking out, and naturally cooling;
the vacuum degree is 0.02 MPa;
the particle size of the diatomite is 30 μm;
(2) uniformly dispersing the heated diatomite into an acid solution, stirring at the rotating speed of 500r/min for 30min, then adjusting the pH of the solution to 9.5, continuing to stir for 1 hour, and then standing for 1 hour to obtain a diatomite dispersion liquid;
the acid solution is a citric acid solution;
the citric acid solution accounts for 5% by mass;
the mixing mass ratio of the diatomite to the citric acid solution is 300 g: 800 mL;
the pH of the adjusting solution is adjusted by adopting a sodium hydroxide solution;
(3) adding calcium chloride accounting for 1.5% of the mass of the diatomite dispersion into the diatomite dispersion, heating to 80 ℃, keeping the temperature and stirring for 30min, then adding rare earth, continuously stirring for 2 hours, then filtering, and drying to constant weight to obtain the diatomite dispersion;
the rare earth is lanthanum chloride;
the mass fraction of lanthanum chloride is 0.002-0.003%;
the drying temperature is 200 ℃;
the acrylic acid copolymer is acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer.
2. The phosphorus-free composite water treatment agent according to claim 1, wherein: the sulfosuccinic acid tetradecyl monoester sulfonate is sulfosuccinic acid tetradecyl monoester sodium sulfonate.
3. The phosphorus-free composite water treatment agent according to claim 1, wherein: the temperature of the water bath is 90-92 ℃;
the ultrasonic treatment frequency is 35kHz, and the power is 500W.
4. The use of the phosphorus-free composite water treatment agent of claim 1 in the field of water treatment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761609A1 (en) * | 1995-08-21 | 1997-03-12 | Kurita Water Industries Ltd. | Anti-scaling terpolymer agent and method for treating water |
| CN103771599A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Phosphorus-free composite scale and corrosion inhibitor and application thereof as well as circulating water treatment method |
| CN106629892A (en) * | 2016-11-25 | 2017-05-10 | 南宁市黑晶信息技术有限公司 | Phosphorus-free corrosion-inhibiting sewage treatment agent for papermaking waste water, and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761609A1 (en) * | 1995-08-21 | 1997-03-12 | Kurita Water Industries Ltd. | Anti-scaling terpolymer agent and method for treating water |
| CN103771599A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Phosphorus-free composite scale and corrosion inhibitor and application thereof as well as circulating water treatment method |
| CN106629892A (en) * | 2016-11-25 | 2017-05-10 | 南宁市黑晶信息技术有限公司 | Phosphorus-free corrosion-inhibiting sewage treatment agent for papermaking waste water, and preparation method thereof |
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