CN111777706A - Preparation method of modified acrylic resin for boiler water treatment - Google Patents
Preparation method of modified acrylic resin for boiler water treatment Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- 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
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/367—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in singly bound form
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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Abstract
The invention discloses a preparation method of modified acrylic resin for boiler water treatment, which comprises the steps of firstly modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid, utilizing a Williamson synthesis method, taking potassium carbonate as an alkali reagent and potassium iodide as a catalyst, adding a proper amount of deoxidant, and reacting 3,4, 5-trihydroxybenzoic acid to obtain 3-allyloxy-4, 5-dihydroxybenzoic acid; then carrying out water solution copolymerization on the 3-allyloxy-4, 5-dihydroxy benzoic acid and acrylic acid or acrylate monomer to obtain modified acrylic resin, and finally adding NaOH to prepare the water treatment agent. The whole preparation process is simple, the preparation cost is low, and the industrial popularization is extremely easy to carry out; the preparation method is only suitable for acrylic acid, has good applicability to acrylate monomers and has wide monomer application range; the prepared efficient scale preventing and removing agent does not contain phosphorus, tannin extract and other carcinogenic substances, is a phosphorus-free, safe and low-cost efficient scale preventing and removing agent, and is green, environment-friendly and pollution-free.
Description
Technical Field
The invention relates to the field of preparation of modified acrylic resin, in particular to a preparation method of modified acrylic resin for boiler water treatment.
Background
The boiler is a device which transfers heat released by fuel combustion to water and generates steam or hot water with certain temperature and pressure, and is widely applied to various departments of modern industry and agriculture and daily life of people. Under the condition of heating evaporation and continuous concentration, the harmful substances entering the boiler along with boiler feed water can be separated out in different forms of precipitates through various physical and chemical processes, and the precipitates can be distinguished into water scales and water residues according to the influence of the precipitates on the boiler. The scale refers to the sediment which is firmly attached to the heated surface, and the crystal of the sediment is hard and compact; the grain slag refers to suspended matters in the boiler water, and is in loose floccule or fine grain shape. The generation of a large amount of water scale and water slag in the boiler causes local heating or corrosion of the boiler body, and irreparable safety accidents can be caused while energy consumption is increased.
The water treatment is to improve the water quality by removing impurities in water through various technologies, or to discharge the impurities in water into water slag to avoid the generation of scale. The boiler water can be added with the medicament, the effects of promoting and reducing the corrosion of the boiler water to a boiler body, promoting the desquamation of water scale, flocculating calcium and magnesium ions, reducing the oxygen content of the boiler water, adjusting the pH value of the boiler water and the like are achieved, the boiler water is indispensable in daily use of a boiler, but the pollution to the environment is caused by the pollution of the existing boiler pollution discharge, and the phosphorus-free water treatment agent becomes an industrial hotspot.
At present, common phosphorus-free water treatment agents comprise inorganic salt, organic treatment agents, tannin extract and the like, wherein the inorganic salt water treatment agents mainly comprise sodium carbonate, sodium hydroxide, silicate, tungstate and molybdate; however, the water treatment agent of the system has limited scale removing capacity, and easily causes overhigh pH value of furnace water and causes alkaline corrosion to a furnace body. The tannin extract water treatment agent mainly comprises tannin and tannic acid, has a good effect of removing water scale, and forms a protective layer on the surface of a furnace body, but in 2017, 10, 27 days, and a reference for preliminary arrangement of a carcinogen list published by the international cancer research institution of the world health organization, tannic acid and tannin are in a 3-class carcinogen list, the existing organic treatment agent mainly comprises polyaspartic acid, polyepoxysuccinic acid and acrylic acid derivatives, compared with polyaspartic acid and polyepoxysuccinic acid, the acrylic acid derivatives have the advantages of low price, easiness in modification and the like, the research status and development of the industrial circulating cooling water scale inhibitor have comprehensive introduction to the acrylic acid derivative treatment agent, mainly polymerization of acrylic acid, acrylamide, maleic acid and itaconic acid, and the defects of few hydroxyl and carboxyl functional groups and the like still exist.
Aiming at the problems in the prior art, the invention utilizes a Williamson synthesis method to graft 3,4,5 trihydroxybenzoic acid into an acrylic resin functional group, and simultaneously increases the number of hydroxyl and carboxyl functional groups in the acrylic resin, thereby obtaining the multi-effect corrosion and scale inhibitor integrating oxygen removal, flocculation and scale removal.
Disclosure of Invention
In order to solve the problems in the prior art, improve the number of hydroxyl and carboxyl functional groups in the acrylic resin, obtain a multi-effect corrosion and scale inhibitor integrating oxygen removal, flocculation and scale removal and solve the problem of pollution of boiler pollution to the environment, the invention provides a preparation method of modified acrylic resin for boiler water treatment.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of modified acrylic resin for boiler water treatment specifically comprises the following steps:
step one, modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid: firstly, dissolving 3,4, 5-trihydroxybenzoic acid with the molar weight of M in acetone, adding the solution into a dry three-neck flask, heating the solution by using a water bath heating device, simultaneously installing a reflux condenser pipe on the three-neck flask for condensation reflux, introducing inert gas nitrogen for protection, and then sequentially adding 1-2.5M mol of allyl chloride, 4M mol of potassium carbonate, 0.2M mol of potassium iodide and 0.2M mol of deoxidant; then reacting and refluxing for 6-12 h in a water bath environment at 60 ℃ under the continuous protection of inert gas nitrogen; finally, carrying out reduced pressure distillation on the obtained product to obtain a 3-allyloxy-4, 5-dihydroxy benzoic acid aqueous solution, and further carrying out extraction, centrifugation and drying to obtain a solid modified sample;
step two, polymerizing 3-allyloxy-4, 5-dihydroxy benzoic acid and a monomer to prepare modified acrylic resin: adding distilled water into a clean and dry three-neck flask, slowly heating until the temperature of the distilled water in the three-neck flask reaches 65 ℃, sequentially and slowly adding a monomer, the solid modified sample obtained in the step one and ammonium persulfate into the distilled water at 65 ℃, uniformly stirring by using a magnetic stirrer, and carrying out condensation reflux, wherein the adding mass ratio of the acrylic monomer, the solid modified sample obtained in the step one and ammonium persulfate is 1: 0.2-0.3: 0.1; the reaction device is provided with a condensation reflux pipe and a temperature measuring meter, the initial temperature of a reaction system is 65 ℃, the temperature of a solution is increased due to heat released in the polymerization process, a reaction liquid gradually refluxes, the reaction system gradually raises the temperature and is stabilized at 90 ℃ for reflux reaction for 0.5-1.0 h, the reaction is completed, the modified acrylic resin is obtained, and the molecular weight of the obtained modified acrylic resin is about 500-1000;
step three, preparation of a water treatment agent: preparing a modified acrylic resin aqueous solution with the mass concentration of 10% by using the obtained modified acrylic resin, and then adding sodium hydroxide to adjust the pH value of the solution to be 12, thereby obtaining the modified acrylic resin water treatment agent capable of being added into boiler water.
In the preparation method of the modified acrylic resin for boiler water treatment, the oxygen scavenger is one of sodium sulfite, potassium sulfite and hydrazine.
The monomer is acrylic acid or acrylate monomer.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the invention provides a preparation method of modified acrylic resin for boiler water treatment, which comprises the steps of firstly modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid, utilizing a Williamson synthesis method, taking potassium carbonate as an alkali reagent and potassium iodide as a catalyst, adding a proper amount of deoxidant, and reacting 3,4, 5-trihydroxybenzoic acid to obtain 3-allyloxy-4, 5-dihydroxybenzoic acid; then copolymerizing the 3-allyloxy-4, 5-dihydroxy benzoic acid and an acrylic acid monomer through an aqueous solution to obtain modified acrylic resin; the whole preparation process is simple, the preparation cost is low, and industrial popularization is extremely easy to carry out;
2. the raw material of the polymerization modified resin is acrylic monomer, but is not limited to acrylic monomer, and can be other acrylic monomers, and the preparation method is proved to have good applicability to the acrylic monomers and wide monomer application range;
3. the efficient scale preventing and removing agent prepared by the preparation method provided by the invention does not contain carcinogens such as tannin extract and the like, is a phosphorus-free, safe and low-cost efficient scale preventing and removing agent, and is green, environment-friendly and pollution-free.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic structural view of a production method in the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
[ example 1 ]
A preparation method of modified acrylic resin for boiler water treatment specifically comprises the following steps:
step one, modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid: firstly, dissolving 3,4, 5-trihydroxybenzoic acid with the molar weight of M in acetone, adding the solution into a dry three-neck flask, heating the solution by using a water bath heating device, simultaneously installing a reflux condenser pipe on the three-neck flask for condensation reflux, introducing inert gas nitrogen for protection, and then sequentially adding M mol of allyl chloride, 4M mol of potassium carbonate, 0.2M mol of potassium iodide and 0.2M mol of sodium sulfite; reacting and refluxing for 12h in a water bath environment at 60 ℃ under the continuous protection of nitrogen; finally, carrying out reduced pressure distillation on the obtained product to obtain a 3-allyloxy-4, 5-dihydroxy benzoic acid aqueous solution, and further carrying out extraction, centrifugation and drying to obtain a solid modified sample;
step two, polymerizing 3-allyloxy-4, 5-dihydroxy benzoic acid and acrylic acid to prepare modified acrylic resin: adding distilled water into a clean and dry three-neck flask, slowly heating until the temperature of the distilled water in the three-neck flask reaches 65 ℃, sequentially and slowly adding an acrylic acid monomer, the solid modified sample obtained in the first step and ammonium persulfate into the distilled water at 65 ℃, uniformly stirring by using a magnetic stirrer, and carrying out condensation reflux, wherein the adding mass ratio of the acrylic acid monomer, the solid modified sample obtained in the first step and ammonium persulfate is 1:0.2: 0.1; the reaction device needs to be provided with a condensation reflux pipe and a temperature measuring meter, the initial temperature of the reaction system is 65 ℃, the temperature of the solution is raised due to the heat released in the polymerization process, the reaction liquid gradually reflows, the temperature of the reaction system is gradually raised and stabilized at 90 ℃ for reflux reaction for 0.5h, the reaction is finished, the modified acrylic resin is obtained, and the molecular weight of the obtained modified acrylic resin is about 500-1000;
step three, preparation of a water treatment agent: preparing a modified acrylic resin aqueous solution with the mass concentration of 10% by using the obtained modified acrylic resin, and then adding sodium hydroxide to adjust the pH value of the solution to be 12, thereby obtaining the modified acrylic resin water treatment agent capable of being added into boiler water.
[ example 2 ]
A preparation method of modified acrylic resin for boiler water treatment specifically comprises the following steps:
step one, modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid: firstly, dissolving 3,4, 5-trihydroxybenzoic acid with the molar weight of M in acetone, adding the solution into a dry three-neck flask, heating the solution by using a water bath heating device, simultaneously installing a reflux condenser pipe on the three-neck flask for condensation reflux, introducing inert gas nitrogen for protection, and then sequentially adding 2.5M mol of allyl chloride, 4M mol of potassium carbonate, 0.2M mol of potassium iodide and 0.2M mol of potassium sulfite; then reacting and refluxing for 6h in a water bath environment at 60 ℃ under the continuous protection of inert gas nitrogen; finally, carrying out reduced pressure distillation on the obtained product to obtain a 3-allyloxy-4, 5-dihydroxy benzoic acid aqueous solution, and further carrying out extraction, centrifugation and drying to obtain a solid modified sample;
step two, polymerizing 3-allyloxy-4, 5-dihydroxy benzoic acid and acrylic acid to prepare modified acrylic resin: adding distilled water into a clean and dry three-neck flask, slowly heating until the temperature of the distilled water in the three-neck flask reaches 65 ℃, sequentially and slowly adding an acrylic acid monomer, the solid modified sample obtained in the first step and ammonium persulfate into the distilled water at 65 ℃, uniformly stirring by using a magnetic stirrer, and carrying out condensation reflux, wherein the adding mass ratio of the acrylic acid monomer, the solid modified sample obtained in the first step and ammonium persulfate is 1:0.3: 0.1; the reaction device is provided with a condensation reflux pipe and a temperature measuring meter, the initial temperature of the reaction system is 65 ℃, the temperature of the solution is increased due to the heat released in the polymerization process, the reaction liquid gradually reflows, the temperature of the reaction system is gradually increased and stabilized at 90 ℃ for reflux reaction for 1.0h, the reaction is finished, the modified acrylic resin is obtained, and the molecular weight of the obtained modified acrylic resin is about 500-1000;
step three, preparation of a water treatment agent: preparing a modified acrylic resin aqueous solution with the mass concentration of 10% by using the obtained modified acrylic resin, and then adding sodium hydroxide to adjust the pH value of the solution to be 12, thereby obtaining the modified acrylic resin water treatment agent capable of being added into boiler water.
[ example 3 ]
A preparation method of modified acrylic resin for boiler water treatment specifically comprises the following steps:
step one, modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid: firstly, dissolving 3,4, 5-trihydroxybenzoic acid with the molar weight of M in acetone, adding the solution into a dry three-neck flask, heating the solution by using a water bath heating device, simultaneously installing a reflux condenser pipe on the three-neck flask for condensation reflux, introducing inert gas nitrogen for protection, and then sequentially adding 1.5M mol of allyl chloride, 4M mol of potassium carbonate, 0.2M mol of potassium iodide and 0.2M mol of hydrazine; then under the continuous protection of inert gas nitrogen, reacting and refluxing for 8h in a water bath environment at 60 ℃; finally, carrying out reduced pressure distillation on the obtained product to obtain a 3-allyloxy-4, 5-dihydroxy benzoic acid aqueous solution, and further carrying out extraction, centrifugation and drying to obtain a solid modified sample;
step two, polymerizing 3-allyloxy-4, 5-dihydroxy benzoic acid and methyl acrylate to prepare modified acrylic resin: adding distilled water into a clean and dry three-neck flask, slowly heating until the temperature of the distilled water in the three-neck flask reaches 65 ℃, sequentially and slowly adding a methyl acrylate monomer, the solid modified sample obtained in the first step and ammonium persulfate into the distilled water at 65 ℃, uniformly stirring by using a magnetic stirrer, and carrying out condensation reflux, wherein the adding mass ratio of the acrylic acid monomer, the solid modified sample obtained in the first step and ammonium persulfate is 1:0.25: 0.1; the reaction device is provided with a condensation reflux pipe and a temperature measuring meter, the initial temperature of the reaction system is 65 ℃, the temperature of the solution is increased due to the heat released in the polymerization process, the reaction liquid gradually reflows, the temperature of the reaction system is gradually increased and stabilized at 90 ℃ for reflux reaction for 40min, the reaction is completed, the modified acrylic resin is obtained, and the molecular weight of the obtained modified acrylic resin is about 500-1000;
step three, preparation of a water treatment agent: preparing a modified acrylic resin aqueous solution with the mass concentration of 10% by using the obtained modified acrylic resin, and then adding sodium hydroxide to adjust the pH value of the solution to be 12, thereby obtaining the modified acrylic resin water treatment agent capable of being added into boiler water.
A large number of tests show that the high-temperature stability of the medicament is good and can be 100-20The scale inhibitor can be stably used in furnace water at 0 ℃, can effectively prevent the generation of new scales and remove old scales, and realizes scale prevention and removal. The hanging piece test proves that: metal corrosion rate < 0.1 g/(m) measured using corrosion indicator chip2H) total corrosion tested < 36g/m2The modified acrylic resin is proved to be capable of forming a good passive film on the surface of metal.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (3)
1. A preparation method of modified acrylic resin for boiler water treatment is characterized by comprising the following steps: the preparation method specifically comprises the following steps:
step one, modifying 3,4, 5-trihydroxybenzoic acid into 3-allyloxy-4, 5-dihydroxybenzoic acid: firstly, dissolving 3,4, 5-trihydroxybenzoic acid with the molar weight of M in acetone, adding the solution into a dry three-neck flask, heating the solution by using a water bath heating device, simultaneously installing a reflux condenser pipe on the three-neck flask for condensation reflux, introducing inert gas nitrogen for protection, and then sequentially adding 1-2.5M mol of allyl chloride, 4M mol of potassium carbonate, 0.2M mol of potassium iodide and 0.2M mol of deoxidant; then reacting and refluxing for 6-12 h in a water bath environment at 60 ℃ under the continuous protection of inert gas nitrogen; finally, carrying out reduced pressure distillation on the obtained product to obtain a 3-allyloxy-4, 5-dihydroxy benzoic acid aqueous solution, and further carrying out extraction, centrifugation and drying to obtain a solid modified sample;
step two, polymerizing 3-allyloxy-4, 5-dihydroxy benzoic acid and a monomer to prepare modified acrylic resin: adding distilled water into a clean and dry three-neck flask, slowly heating until the temperature of the distilled water in the three-neck flask reaches 65 ℃, sequentially and slowly adding a monomer, the solid modified sample obtained in the step one and ammonium persulfate into the distilled water at 65 ℃, uniformly stirring by using a magnetic stirrer, and carrying out condensation reflux, wherein the adding mass ratio of the acrylic monomer, the solid modified sample obtained in the step one and ammonium persulfate is 1: 0.2-0.3: 0.1; the reaction device is provided with a condensation reflux pipe and a temperature measuring meter, the initial temperature of a reaction system is 65 ℃, the temperature of a solution is raised due to heat release of polymerization, a reaction liquid is gradually refluxed, the reaction system is gradually heated and is stabilized at 90 ℃ for reflux reaction for 0.5-1.0 h, the reaction is finished, the modified acrylic resin is obtained, and the molecular weight of the obtained modified acrylic resin is about 500-1000;
step three, preparation of a water treatment agent: and (3) preparing a modified acrylic resin aqueous solution with the mass concentration of 10% by using the modified acrylic resin obtained in the second step, and then adding sodium hydroxide to adjust the pH value of the solution to 12, so as to obtain the modified acrylic resin water treatment agent capable of being added into boiler water.
2. The preparation method of the modified acrylic resin for boiler water treatment according to claim 1, wherein the oxygen scavenger is one of sodium sulfite, potassium sulfite and hydrazine.
3. The preparation method of the modified acrylic resin for boiler water treatment as claimed in claim 1, wherein the monomer is acrylic acid or acrylate monomer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114621647A (en) * | 2022-05-12 | 2022-06-14 | 佛山市三水联美化工有限公司 | Polyurethane resin coating and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110281115A1 (en) * | 2010-05-13 | 2011-11-17 | Kania Charles M | Curable film-forming compositions containing ortho-hydroxyl aromatic functional acrylic polymers |
| CN102616946A (en) * | 2011-06-23 | 2012-08-01 | 陕西省石油化工研究设计院 | Biodegradable corrosion and scale inhibitor epoxy succinic acid copolymer and its preparation method |
| CN104944601A (en) * | 2015-06-05 | 2015-09-30 | 东南大学 | Environment-friendly polyether water treatment agent and preparation method thereof |
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2020
- 2020-06-06 CN CN202010508662.5A patent/CN111777706B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110281115A1 (en) * | 2010-05-13 | 2011-11-17 | Kania Charles M | Curable film-forming compositions containing ortho-hydroxyl aromatic functional acrylic polymers |
| CN102616946A (en) * | 2011-06-23 | 2012-08-01 | 陕西省石油化工研究设计院 | Biodegradable corrosion and scale inhibitor epoxy succinic acid copolymer and its preparation method |
| CN104944601A (en) * | 2015-06-05 | 2015-09-30 | 东南大学 | Environment-friendly polyether water treatment agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621647A (en) * | 2022-05-12 | 2022-06-14 | 佛山市三水联美化工有限公司 | Polyurethane resin coating and preparation method and application thereof |
| CN114621647B (en) * | 2022-05-12 | 2022-08-05 | 佛山市三水联美化工有限公司 | Polyurethane resin coating and preparation method and application thereof |
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