CN112093918B - Humic acid phosphorus-free corrosion and scale inhibitor and preparation method thereof - Google Patents
Humic acid phosphorus-free corrosion and scale inhibitor and preparation method thereof Download PDFInfo
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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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
- C02F5/105—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 combined with inorganic substances
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a humic acid phosphorus-free corrosion and scale inhibitor. The corrosion and scale inhibitor adopts active humic acid and humic acid zwitterionic dispersant, has chelation effect on metal ions, has dispersion effect on calcium carbonate and calcium phosphate, can form soft and non-wall-hanging soft scale, and simultaneously forms good synergistic effect with the active humic acid and humic acid zwitterionic dispersant and various auxiliary components, thereby reducing the dosage of the composite scale inhibitor. The scale inhibitor is used for circulating water of a power plant, has the functions of sterilization and bacteriostasis, is environment-friendly due to no phosphorus, can be biologically decomposed, and is a green environment-friendly composite scale inhibitor.
Description
Technical Field
The invention relates to the field of circulating water corrosion and scale inhibitors for power plants, in particular to a humic acid phosphorus-free corrosion and scale inhibitor and a preparation method thereof.
Background
Circulating water is transmitted through a heat exchanger, an open cooling tower and pipelines with different lengths of the system, and then a series of changes such as temperature change, evaporative concentration, rich oxidation and the like can occur, so that system equipment is corroded and scaled, the heat transfer effect is reduced, and the equipment is consumed. In order to achieve the purposes of saving water and energy and prolonging the service life of system equipment, two problems of corrosion and scaling of a circulating cooling water system must be solved, and adding a corrosion inhibitor into a corrosion medium and reducing the corrosion rate of metal are the most common solutions. The reason why the composite corrosion inhibitor is used in large quantities is that it utilizes the synergistic effect among the corrosion inhibitors to improve the adsorption coverage and the adsorption stability, change the adsorption speed, reduce the dosage of the corrosion inhibitor and reduce the toxicity of the corrosion inhibitor. The single-agent corrosion inhibitor can be compounded to prepare the composite corrosion inhibitor with higher corrosion inhibition efficiency, thereby expanding the application range of the corrosion inhibitor and solving the difficulty which is difficult to overcome by single-component corrosion inhibitors.
In recent years, the application development of the organic phosphoric acid corrosion and scale inhibitor is extremely rapid, and the common corrosion and scale inhibitors for domestic circulating cooling water treatment comprise polyphosphate, phosphoric acid vinegar, organic phosphoric acid, polymers and the like. The organic phosphoric acid medicament is widely applied by the double functions of high-efficiency corrosion inhibition and scale inhibition, and the water treatment medicament has the characteristics of stable chemical performance, high temperature and value resistance, obvious solution limit effect and synergistic effect and the like. However, phosphorus is a nutrient source of bacteria and algae, and the phosphorus-containing scale inhibitor is easy to cause eutrophication of environmental water areas and promote the growth of bacteria and algae to form red tide to cause water source pollution. The phosphorus-free corrosion and scale inhibitor has the advantages of environmental protection and low corrosion and scale inhibition effect, particularly has unstable medicament effect and is easy to absorb and consume under poor water quality conditions, and the corrosion and scale inhibition performance is greatly influenced. Therefore, the development of a novel green corrosion and scale inhibitor which is phosphorus-free, has good biodegradation performance, simple and easily realized control index and is suitable for high-concentration-ratio operation and even zero pollution discharge has become a development direction of water treatment.
Disclosure of Invention
One of the purposes of the invention is to provide the humic acid non-phosphorus corrosion and scale inhibitor which is green and environment-friendly, easy to biodegrade, high in corrosion inhibition performance and high in scale inhibition performance, can be used in a circulating water system with reuse water as make-up water, is particularly suitable for circulating water with total iron of more than or equal to 1mg/L, has a synergistic effect on all components, and is stable in use effect and excellent in corrosion and scale inhibition performance.
In order to achieve the purpose, the invention provides the following technical scheme: the corrosion and scale inhibitor comprises humic acid derivatives containing phenolic hydroxyl, carboxyl and quinonyl, a corrosion inhibitor, a synergistic agent and a solvent; the solvent is an aqueous solution of methanol.
The composition comprises, in parts by weight,
100 portions of humic acid derivative A liquid and 500 portions of humic acid derivative A liquid;
100-500 parts of humic acid zwitterionic compound B liquid;
60-130 parts of a corrosion inhibitor;
60-190 parts of a synergistic agent;
100 portions of methanol and 300 portions.
The humic acid derivative A liquid comprises 60 parts of humic acid, 20 parts of an oxidant and 3 parts of a catalyst; preferably, the humic acid is ammonium humate; preferably, the oxidant is hydrogen peroxide with the mass concentration of 30%; preferably, the catalyst is a catalyst comprising copper ions and iron ions; preferably, the catalyst is a mixture of ferric sulfate and copper sulfate in a weight ratio of (4-10) to (2-6); preferably, the weight ratio of the ferric sulfate to the copper sulfate is 7: 4.
the humic acid zwitterionic compound B liquid comprises 1 part of ionic monomer solution, 200 parts of humic acid derivative A liquid, 3 parts of initiator and 3 parts of terminator; preferably, the ionic monomer solution is a mixed solution of dimethyl diallyl chloride and allyl sulfonate; preferably, the mass ratio of the dimethyl diallyl chloride salt to the allyl sulfonate is 3-10; preferably, the ionic monomer mixed solution is a mixed solution of dimethyl diallyl ammonium chloride and sodium allyl sulfonate; preferably, the ionic monomer solution is a mixed solution of 3 parts of 60 mass percent dimethyldiallylammonium chloride solution and 10 parts of sodium allylsulfonate dissolved in 50 parts of water; preferably, the initiator is potassium persulfate solution; the terminator is sodium carbonate.
Preferably, the corrosion inhibitor is sodium nitrite (NaNO)4) Mixing with Benzotriazole (BTA); preferably, the NaNO450-100 parts of BTA, 10-30 parts of BTA;
preferably, the synergistic agent is a mixture of thiourea compound and inorganic potassium salt; preferably, the thiourea compound is thiourea; preferably, the inorganic potassium salt is potassium iodide; preferably, the thiourea is 10-40 parts, and the potassium iodide is 50-150 parts;
the invention also aims to provide a preparation method of the scale inhibitor, which takes humic acid as a raw material, and catalytically oxidizes the humic acid into humic acid derivatives rich in phenolic hydroxyl, carboxyl and quinonyl groups as active humic acid; mixing the active humic acid and the ionic monomer, and synthesizing the zwitterionic macromolecular dispersant by graft copolymerization of free radicals under the action of an initiator; the active humic acid and the zwitterionic macromolecular dispersant thereof are mixed with a corrosion inhibitor, a synergistic agent and a solvent to prepare the phosphorus-free corrosion and scale inhibitor.
The method comprises the following specific steps:
s1, preparing active humic acid: adding humate, an oxidant and a catalyst into a solvent, stirring and mixing, and controlling a certain pressure and temperature to perform an oxidation reaction; concentrating under reduced pressure to obtain humic acid derivative A solution;
s2, preparing a dispersing agent: preparing an ionic monomer solution at normal temperature and normal pressure, sequentially adding the humic acid derivative A solution obtained in the step S1 and an initiator, and adding a terminator after graft copolymerization reaction for a period of time to obtain a humic acid zwitterionic compound B solution;
s3, preparing a corrosion and scale inhibitor: mixing the humic acid derivative A liquid, the humic acid zwitterionic compound B liquid, the corrosion inhibitor, the synergistic agent and the solvent, and uniformly stirring to obtain the target product.
In an embodiment of the present invention, in step S1, the oxidizing agent is hydrogen peroxide with a mass concentration of 30%.
As an embodiment of the present invention, in step S1, the catalyst is a metal catalyst; preferably, the catalyst is a catalyst comprising copper ions and iron ions; preferably, the catalyst is a mixture of ferric sulfate and copper sulfate; preferably, the catalyst is a mixture of ferric sulfate and copper sulfate in a weight ratio of (4-10) to (2-6).
As an embodiment of the present invention, in step S1, the reaction pressure is 4 to 8 atmospheres; and/or the reaction temperature is 40-110 ℃; and/or the reaction time is 4 to 12 hours.
As an embodiment of the present invention, in step S2, the ionic monomer solution is a mixed solution of dimethyl diallyl chloride and allyl sulfonate; preferably, the weight ratio of the dimethyl diallyl chloride to the allyl sulfonate is (1-3) to (8-12); preferably, the ionic monomer solution is a mixed solution of dimethyl diallyl ammonium chloride and sodium allyl sulfonate.
As an embodiment of the present invention, in step S2, the initiator is a potassium persulfate solution; and/or the terminating agent is sodium carbonate.
As an embodiment of the present invention, in step S2, the reaction temperature of the polymerization reaction is 50 to 95 ℃; and/or the reaction time is 0.5 to 3 hours.
As an embodiment of the present invention, in step S3, 100 parts by weight of the humic acid derivative A liquid is 500 parts; 100-500 parts of humic acid zwitterionic compound B liquid; 60-130 parts of a corrosion inhibitor; 60-190 parts of synergistic agent; 100 portions of methanol and 300 portions.
In step S3, the corrosion inhibitor is sodium nitrite (NaNO)4) Compatible with Benzotriazole (BTA), preferably, the NaNO450-100 parts of BTA, 10-30 parts of BTA; and/or the synergistic agent is a mixture of thiourea and inorganic potassium salt; preferably, the inorganic potassium salt is potassium iodide; preferably, the thiourea is 10-40 parts, and the potassium iodide is 50-150 parts.
As an embodiment of the present invention, in step S3, the solvent is a mixed solvent of methanol and water; preferably, the methanol content is 100-300 parts.
The invention also aims to provide the application of the humic acid phosphorus-free corrosion and scale inhibitor in circulating water treatment. Is particularly suitable for circulating water with calcium ions more than or equal to 1mg/L, and is further used for treating circulating water of a power plant.
The fourth purpose of the invention is to provide a method for treating circulating water, which comprises adding the humic acid phosphorus-free corrosion and scale inhibitor into the circulating water. Furthermore, the amount of the humic acid slow-release scale inhibitor added into each 1L of circulating water is 3-20 mL.
As an embodiment of the invention, the dosage of the humic acid slow-release scale inhibitor added into every 1L of circulating water is 10 mL.
The technical scheme provided by the invention has the beneficial effects that at least:
the humic acid phosphorus-free corrosion and scale inhibitor provided by the invention adopts the active humic acid and humic acid zwitterionic dispersing agent, has a chelation effect on metal ions, has a dispersing effect on calcium carbonate and calcium phosphate, can form soft and wall-hanging-free soft scale, and simultaneously forms a good synergistic effect with each auxiliary component by the active humic acid and humic acid zwitterionic dispersing agent, so that the dosage of the composite scale inhibitor is reduced. The scale inhibitor provided by the invention is green and environment-friendly, is easy to biodegrade, has high corrosion inhibition and high scale inhibition, can be used in a circulating water system with recycled water as make-up water, is particularly suitable for circulating water with calcium ions of more than or equal to 1mg/L, has sterilization and bacteriostasis effects, has a synergistic effect on each component, is stable in use effect, can be biodegraded, and has excellent corrosion and scale inhibition performance.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
[ example 1 ] preparation of humic acid derivative A solution
Adding 60g of ammonium humate into 300g of distilled water, stirring and dissolving, filtering, adding the filtrate into a sealed high-pressure kettle, simultaneously adding 3g of catalyst into the sealed high-pressure kettle, sealing by 20g of hydrogen peroxide with the mass concentration of 30%, maintaining the temperature of 80 ℃ and the pressure of 4 atmospheric pressures in a stirring state, reacting for 8 hours, and concentrating until the solid content is 12% to obtain a humic acid derivative A liquid.
The catalyst is a mixture of ferric sulfate and copper sulfate in a weight ratio of 7: 4.
[ example 2 ] preparation of humic acid zwitterionic compound B solution
200mL of humic acid derivative A liquid prepared in example 1 was heated to 74 ℃ and added to a monomer solution, followed by addition of an initiator, reaction time 1.5 hours and addition of 0.5g of sodium carbonate as a terminator to obtain humic acid zwitterionic compound B liquid.
The monomer solution is 3g of dimethyldiallylammonium chloride solution with the mass concentration of 60% dissolved in 50mL of pure water and 10g of sodium allylsulfonate.
The initiator was prepared by dissolving 2.5g of potassium persulfate in 50mL of pure water.
Example 3 preparation of humic acid phosphorus-free corrosion and scale inhibitor
300mL of the humic acid derivative A solution prepared in example 1, 300mL of the humic acid zwitterionic compound B solution prepared in example 2, and NaNO4100g of humic acid phosphorus-free corrosion and scale inhibitor is obtained by mixing 100g of BTA 20g of thiourea, 100g of potassium iodide and 200g of methanol at normal temperature and uniformly stirring.
Example 4 preparation of humic acid phosphorus-free corrosion and scale inhibitor
400mL of the humic acid derivative A solution prepared in example 1, 400mL of the humic acid zwitterionic compound B solution prepared in example 2, and NaNO4100g of humic acid phosphorus-free corrosion and scale inhibitor is obtained by mixing 100g of BTA 20g of thiourea, 100g of potassium iodide and 200g of methanol at normal temperature and uniformly stirring.
Example 5 preparation of humic acid phosphorus-free corrosion and scale inhibitor
200mL of humic acid derivative A solution prepared in example 1, 200mL of humic acid zwitterionic compound B solution prepared in example 2, and NaNO4100g of humic acid phosphorus-free corrosion and scale inhibitor is obtained by mixing 100g of BTA 20g of thiourea, 100g of potassium iodide and 200g of methanol at normal temperature and uniformly stirring.
Example 6 preparation of humic acid phosphorus-free corrosion and scale inhibitor
100mL of the humic acid derivative A solution prepared in example 1, 100mL of the humic acid zwitterionic compound B solution prepared in example 2, and NaNO4100g of humic acid phosphorus-free corrosion and scale inhibitor is obtained by mixing 100g of BTA 20g of thiourea, 100g of potassium iodide and 200g of methanol at normal temperature and uniformly stirring.
[ COMPARATIVE EXAMPLE ] PREPARATION OF COMMON SCALE-RESISTANT AGENT
5g of sodium metasilicate pentahydrate, 10g of sodium polyacrylate, NaNO 4100 g, 20g of BTA, 20g of thiourea, 100g of potassium iodide and 200g of methanol are mixed at normal temperature and uniformly stirred to obtain the humic acid phosphorus-free corrosion and scale inhibitor.
The scale and corrosion inhibition rates of examples 3 to 6 and comparative examples were determined according to the execution Standard HG/T2431-2018. The water for testing is prepared according to the preparation of the A.2 standard configuration water in the appendix A of GB/T18175-2014 water treatment agent corrosion inhibition performance measurement spin hanging sheet method. Wherein, the amount of the humic acid slow-release scale inhibitor added into each 1L of test water is 10mL according to the above examples 3-6 and comparative examples. Specific results are shown in table 1.
TABLE 1
| Serial number | Scale inhibition rate/%) | Inhibition rate/%) |
| Example 3 | 99.5 | 99.1 |
| Example 4 | 99.2 | 98.8 |
| Example 5 | 98.0 | 98.3 |
| Example 6 | 97.6 | 98.1 |
| Comparative example | 85.7 | 93.2 |
As can be seen from the data in table 1: the main reason is that the active humic acid and humic acid zwitterionic dispersant is adopted, has chelation effect on metal ions, has dispersion effect on calcium carbonate and calcium phosphate, can form soft and non-wall-hanging soft scale, and simultaneously forms good synergistic effect with each auxiliary component.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (7)
1. A humic acid phosphorus-free corrosion and scale inhibitor is characterized in that: the corrosion and scale inhibitor comprises humic acid derivatives containing phenolic hydroxyl, carboxyl and quinonyl, a corrosion inhibitor, a synergistic agent and a solvent; the solvent is an aqueous solution of methanol;
based on the parts by weight, the weight ratio,
100 portions of humic acid derivative A liquid and 500 portions of humic acid derivative A liquid;
100-500 parts of humic acid zwitterionic compound B liquid;
60-130 parts of a corrosion inhibitor; the corrosion inhibitor is sodium nitrite (NaNO)4) Mixing with Benzotriazole (BTA); the NaNO450-100 parts of BTA, 10-30 parts of BTA;
60-190 parts of a synergistic agent; the synergistic agent is a mixture of thiourea compounds and inorganic potassium salt; the thiourea compound is thiourea; the inorganic potassium salt is potassium iodide; 10-40 parts of thiourea and 50-150 parts of potassium iodide;
100 portions of methanol and 300 portions;
the humic acid derivative A liquid comprises 60 parts of ammonium humate, 20 parts of an oxidant and 3 parts of a catalyst; the oxidant is hydrogen peroxide with the mass concentration of 30%; the catalyst is a catalyst comprising copper ions and iron ions; the weight ratio of the catalyst is 7: 4, a mixture of ferric sulfate and copper sulfate;
the humic acid zwitterionic compound B liquid comprises 1 part of ionic monomer solution, 200 parts of humic acid derivative A liquid, 3 parts of initiator and 3 parts of terminator; the ionic monomer solution is a mixed solution prepared by dissolving 3 parts of 60 mass percent dimethyl diallyl ammonium chloride solution and 10 parts of sodium allylsulfonate in 50 parts of water; the initiator is potassium persulfate solution; the terminator is sodium carbonate.
2. A method for preparing the humic acid phosphorus-free corrosion and scale inhibitor according to claim 1, which is characterized by comprising the following steps: the method comprises the specific steps of carrying out,
s1 preparation of active humic acid: adding humate, an oxidant and a catalyst into a solvent, stirring and mixing, and controlling a certain pressure and temperature to perform an oxidation reaction; then, concentrating under reduced pressure to obtain humic acid derivative A liquid;
s2 dispersant preparation: preparing an ionic monomer solution at normal temperature and normal pressure, sequentially adding the humic acid derivative A solution obtained in the step S1 and an initiator, and adding a terminator after a polymerization reaction is carried out for a period of time to obtain a humic acid zwitterionic compound B solution; the initiator is potassium persulfate solution; the terminator is sodium carbonate; the reaction temperature of the polymerization reaction is 50-95 ℃; the reaction time is 0.5 to 3 hours;
s3, preparing a corrosion and scale inhibitor: mixing humic acid derivative A liquid, humic acid zwitterionic compound B liquid, corrosion inhibitor, synergistic agent and solvent, and stirring uniformly to obtain a target product; the solvent is a mixed solvent of methanol and water; the methanol content is 100-300 portions.
3. The preparation method of the humic acid phosphorus-free corrosion and scale inhibitor according to claim 2, which is characterized by comprising the following steps: in step S1, the reaction pressure is 4-10 atmospheres; the reaction temperature is 40-110 ℃; the reaction time is 4-12 hours.
4. The application of the humic acid phosphorus-free corrosion and scale inhibitor of claim 1 in the treatment of circulating water; is suitable for circulating water with calcium ion not less than 1 mg/L.
5. The application of the humic acid phosphorus-free corrosion and scale inhibitor in circulating water treatment according to claim 4 is characterized in that: the method is used for treating the circulating water of the power plant.
6. The application of the humic acid phosphorus-free corrosion and scale inhibitor in the treatment of circulating water according to claim 4 is characterized in that: the humic acid phosphorus-free corrosion and scale inhibitor is added into circulating water; the amount of the humic acid slow-release scale inhibitor added into each 1L of circulating water is 3-20 mL.
7. The application of the humic acid non-phosphorus corrosion and scale inhibitor in the treatment of circulating water according to claim 6 is characterized in that: the dosage of the humic acid slow-release scale inhibitor added into each 1L of circulating water is 10 mL.
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| CN110862495A (en) * | 2019-11-12 | 2020-03-06 | 句容宁武高新技术发展有限公司 | Multifunctional phosphorus-free corrosion and scale inhibitor based on humic acid derivatives and preparation method thereof |
| CN114408900B (en) * | 2022-02-18 | 2023-07-14 | 自然资源部第二海洋研究所 | Method for preparing carbon nano particles by using humic acid and application |
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