CN103031559B - Preparation of pH-controlled-release long-acting intelligent corrosion inhibitor - Google Patents
Preparation of pH-controlled-release long-acting intelligent corrosion inhibitor Download PDFInfo
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- CN103031559B CN103031559B CN201310004233.4A CN201310004233A CN103031559B CN 103031559 B CN103031559 B CN 103031559B CN 201310004233 A CN201310004233 A CN 201310004233A CN 103031559 B CN103031559 B CN 103031559B
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Abstract
The invention belongs to the field of preparation of intelligent corrosion inhibitors, and particularly relates to a preparation method of a pH-controlled-release long-acting intelligent corrosion inhibitor. A using method of the conventional corrosion inhibitor is realized mainly through one-time addition or continuous addition for multiple times, and the concentration of the corrosion inhibitor in an early period is too high, while the concentration of the corrosion inhibitor in a late period is too low, therefore, resource waste is caused, the slow release efficiency is reduced, and even sometimes, the corrosion rate is accelerated, as a result, the invention prepares the pH-controlled-release long-acting intelligent corrosion inhibitor which is a hydrogel-embedded corrosion inhibitor, is sensitive to ambient pH and has a corrosion inhibiting function; and the intelligent corrosion inhibitor can determine the release condition according to different properties of an ambient medium.
Description
Technical field
The invention belongs to the preparation field of intelligent inhibiter, particularly a kind of can by pH Co ntrolled release long-acting type intelligence inhibiter preparation method.
Background technology
The every field of metallic corrosion in life is produced, and the method for minimizing or prevention metallic corrosion is also diversified.Wherein, inhibiter relies on easy, quick, the economic dispatch advantage of its using method and is widely used.But mostly the using method of traditional inhibiter is to adopt once throws in or continuous several times input, this just made at the input initial stage, and density of corrosion inhibitor is too high, even higher than the highest effective concentration, this is not only the waste of resource, sometimes also can reduce the even accelerated corrosion of slowly-releasing efficiency.In the input later stage, density of corrosion inhibitor is too low, even lower than minimal effective concentration, thus reduces inhibition efficiency, also shortens the work-ing life of inhibiter simultaneously.Therefore, both at home and abroad investigator is devoted to research always and obtains a kind of intelligent long-acting inhibiter for many years, expects that this inhibiter can according to surrounding environment change, automatically control the release conditions of inhibiter and burst size number.The hydrogel of nontoxic, the free of contamination pH of having susceptibility is applied to the carrier as inhibiter in intelligent inhibiter, is one of direction of future studies intelligence inhibiter.
Usually containing ionogen in the macromolecular skeleton chain of pH sensitive aqueous gel, as hydroxy-acid group or amino group etc.Because these groups can produce ionization in various degree/protonated along with the change of surrounding medium pH value, hydrogel internal penetration is pressed and ionic linkage reactive force changes, thus cause volume that swelling change occurs, demonstrate pH susceptibility.For the pH sensitive aqueous gel of band slightly acidic group, if surrounding medium pH value is greater than the ionization equilibrium constant (pKa) of slightly acidic group, slightly acidic group ionization then on hydrogel molecules chain side chain forms charged negatively charged ion, thus produce larger osmotic pressure in hydrogel inside, simultaneously because interionic interaction repulsion increases, it is swelling that this all makes hydrogel occur.Same reason, the hydrogel of band weakly alkaline group produces swelling when then surrounding medium pH value is less than its ionization equilibrium constant pKa.
Based on pH sensitive aquagel, there is this responsiveness to environmental pH, inhibiter can be embedded in this hydrogel, controlling the release performance of the inhibiter be embedded in wherein by controlling the swelling of such hydrogel and deswelling degree further.Because mostly the pH sensitive aquagel of synthesis is environmental protection, nontoxic high molecular polymer, therefore the toxicity of this kind of inhibiter is little, few to the harm of human body and environment.
The size of pH sensitive aquagel response environment pH value change generation volume change and pH responsive thereof are the Key Performance Indicators of this kind of intelligent aqueous gel capable.PH responsive is higher, and it is more favourable in inhibiter controllable release as inhibiter carrier.Swelling property is better, and the amount of its inhibiter that can embed is larger.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of can by the preparation method of the long-acting type intelligence inhibiter of pH Co ntrolled release, the method technique is simple, and cost is low, is widely used.The long-acting intelligent inhibiter long service life of preparation, corrosion mitigating effect is good, has a good application prospect.
In order to solve existing issue, technical scheme provided by the invention is:
A kind of can by the preparation method of the long-acting intelligent inhibiter of pH Co ntrolled release, be 5%-10% by the macromolecular material content with three-dimensional network, monomer content is 5%-10%, initiator content is 0.01-0.1 times of monomer, content of crosslinking agent is 0.01-0.1 times of monomer mass, Content of Pore-forming Agents is 0.05%-0.15%, inhibiter content is 5-15mg/mL composition, described three-dimensional network high molecular polymer is one of starch or chitosan, described monomer is vinylformic acid, one of methacrylic acid or hydroxyethyl methylacrylate, described linking agent is one of methylene-bisacrylamide or four condensed ethandiol double methacrylates, described initiator is one of ammonium persulphate or Potassium Persulphate, described pore forming material is one of sodium bicarbonate or acetone, its preparation method includes following steps:
1) preparation of the hydrogel of pH response
A the high molecular polymer with three-dimensional net structure is placed in the there-necked flask with prolong, agitator and thermometer by (), the deionized water adding 20-40mL is mixed with the aqueous solution, pass into nitrogen and Keep agitation, stirring velocity is 200-500 rev/min, keep being warming up to 60-100 DEG C, then in aqueous solutions of polymers, add initiator, reaction for some time after add monomer and linking agent, and under 60-100 DEG C of constant temperature sustained reaction 60-180min.
B () reaction terminates after, be cooled to room temperature, and regulate pH with one of NaOH aqueous solution of HCl or 1M of 1M, add pore forming material, and uniform stirring; Products therefrom is poured in ethanol and cleans, after leaving standstill 3-5h, ethanol is poured out, product is put into loft drier dry, obtain xerogel.
2) preparation of the long-acting intelligent inhibiter of pH Co ntrolled release
Described hydrogel is dissolved in the dry solution containing inhibiter, soaks 2-4 days, filter, and through vacuum lyophilization, can obtain can by the long-acting intelligent inhibiter of pH Co ntrolled release.
Another technical scheme of the present invention is above-mentioned inhibiter is one of benzotriazole (BTA), imidazolines, imidazolidine derivatives.
The long-acting type intelligence inhibiter of pH Co ntrolled release prepared by the present invention by changing the pH value of surrounding medium, high molecular polymer and the consumption of monomer, the consumption of linking agent to regulate pore size and the swelling capacity size of pH sensitive aquagel, thus can control embedding amount and the burst size of inhibiter.
Beneficial effect of the present invention:
(1) present invention process is simple, and cost is low, adopts and use water as reaction medium in preparation process, produces without poisonous and hazardous by product, environmentally friendly;
(2) the pH responsiveness of long-acting type intelligence inhibiter to surrounding medium of the pH Co ntrolled release prepared of the present invention is good, the cycle in work-ing life is long, inhibition efficiency is high, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the long-acting type intelligence swelling property of inhibiter and the relation curve of medium pH of the pH Co ntrolled release of preparation.
Fig. 2 is the pH sensitivity tests curve of the long-acting type intelligence inhibiter of the pH Co ntrolled release of preparation.
Fig. 3 is the inhibiter release kinetics profile of the long-acting type intelligence inhibiter of the pH Co ntrolled release of preparation.
Fig. 4 be pH Co ntrolled release long-acting type intelligence inhibiter and traditional inhibiter deposit in case, the electrochemical tests of 7A04Al.
Fig. 5 be pH Co ntrolled release long-acting type intelligence inhibiter and traditional inhibiter deposit in case, the ac impedance spectroscopy of 7A04.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read content of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
1) preparation of the hydrogel of pH sensitivity
A) joining in the there-necked flask with prolong, agitator and thermometer by 2.0g starch, adding 35mL distilled water, passing into nitrogen, stirring velocity is 300 revs/min, is warming up to 80 DEG C gradually.0.1g ammonium persulfate initiator is dissolved in 5mL deionized water, is joining in above-mentioned reactant aqueous solution, maintaining nitrogen purge, stable reaction 10min.1.5g vinylformic acid and 1.5g hydroxyethyl methylacrylate are joined in above-mentioned reactant aqueous solution; 0.05g methylene-bisacrylamide linking agent is same as in 5mL deionized water, joins in above-mentioned reactant aqueous solution, control to react 60min under above-mentioned stirring velocity and temperature.
B), after reaction terminates, room temperature is cooled to, and with the NaOH solution adjust pH to 8 of 1M.Add 0.05g sodium bicarbonate whipping agent, stirring velocity is 500 revs/min, to producing uniform form of foam.The hydrogel of gained is injected excessive ethanol, leaves standstill 3h; By ethanol everywhere, and product is cut into small pieces, then adds 100mL ethanol, and leave standstill 24h.Finally by with the gel filtered in drying machine, at 60 DEG C, dry 10h, grinds product with mortar, is preserved by powder-tight, lucifuge, to be Protected from Heat.
2) preparation of the long-acting type intelligence inhibiter of pH Co ntrolled release
The pH be dissolved in by the dry gel powder of above-mentioned for 0.1g gained containing benzo three nitrogen file (BTA) inhibiter is in the aqueous solution of 8, BTA concentration is 5mg/mL, leave standstill 48 hours, gained is carried inhibiter hydrogel washed with de-ionized water three times, after vacuum lyophilization, grind into powder sealing preserve, for subsequent use.
Performance test being carried out to the long-acting type intelligence inhibiter of obtained pH Co ntrolled release: by by 1) obtained pH response water gel is dissolved in the aqueous solution of different pH value, leave standstill 30min, measure its swelling front and back quality, obtain the swelling property of pH response water gel and the relation curve of medium pH, as shown in Figure 1.By by 1) obtained pH response water gel is alternately dissolved in the solution of pH2 and pH8, obtains the pH sensitivity tests curve of pH response water gel, as shown in Figure 2.By by 2) the long-acting type intelligence inhibiter of pH Co ntrolled release that obtains is dissolved in the aqueous solution of pH 8, obtains the release kinetics profile of this inhibiter, as shown in Figure 3.7A04 aluminium alloy is immersed in respectively containing pH Co ntrolled release long-acting type intelligence inhibiter and traditional inhibiter 3.5%NaCl solution in, measure its electrochemical tests and ac impedance spectroscopy after 3h and 5h, acquired results is as shown in Figures 4 and 5.
Embodiment 2
1) preparation of the hydrogel of pH sensitivity
A) joining in the there-necked flask with prolong, agitator and thermometer by 1.0g starch, adding 10mL distilled water, passing into nitrogen, stirring velocity is 300 revs/min, is warming up to 70 DEG C gradually.0.03g ammonium persulfate initiator is dissolved in 3mL deionized water, is joining in above-mentioned reactant aqueous solution, maintaining nitrogen purge, stable reaction 10min.1g vinylformic acid and 1g hydroxyethyl methylacrylate are joined in above-mentioned reactant aqueous solution; 0.03g methylene-bisacrylamide linking agent is same as in 3mL deionized water, joins in above-mentioned reactant aqueous solution, control to react 100min under above-mentioned stirring velocity and temperature.
B), after reaction terminates, room temperature is cooled to, and with the NaOH solution adjust pH to 8 of 1M.Add 0.05g sodium bicarbonate whipping agent, stirring velocity is 500 revs/min, to producing uniform form of foam.The hydrogel of gained is injected excessive ethanol, leaves standstill 3h; By ethanol everywhere, and product is cut into small pieces, then adds 100mL ethanol, and leave standstill 24h.Finally by with the gel filtered in drying machine, at 60 DEG C, dry 10h, grinds product with mortar, is preserved by powder-tight, lucifuge, to be Protected from Heat.
2) preparation of the long-acting type intelligence inhibiter of pH Co ntrolled release
Be in the aqueous solution of 8 by the dry gel powder of above-mentioned for the 0.1g gained pH be dissolved in containing BTA inhibiter, benzotriazole (BTA) concentration is 5mg/mL, leave standstill 48 hours, gained is carried inhibiter hydrogel washed with de-ionized water three times, after vacuum lyophilization, grind into powder sealing preserve, for subsequent use.
Embodiment 3
1) preparation of the hydrogel of pH sensitivity
A) joining in the there-necked flask with prolong, agitator and thermometer by 2.0g starch, adding 20mL distilled water, passing into nitrogen, stirring velocity is 300 revs/min, is warming up to 100 DEG C gradually.0.3g ammonium persulfate initiator is dissolved in 5mL deionized water, is joining in above-mentioned reactant aqueous solution, maintaining nitrogen purge, stable reaction 10min.1.5g vinylformic acid and 1.5g hydroxyethyl methylacrylate are joined in above-mentioned reactant aqueous solution; 0.3g methylene-bisacrylamide linking agent is same as in 5mL deionized water, joins in above-mentioned reactant aqueous solution, control to react 150min under above-mentioned stirring velocity and temperature.
B), after reaction terminates, room temperature is cooled to, and with the NaOH solution adjust pH to 8 of 1M.Add 0.05g sodium bicarbonate whipping agent, stirring velocity is 500 revs/min, to producing uniform form of foam.The hydrogel of gained is injected excessive ethanol, leaves standstill 3h; By ethanol to going out, and product is cut into small pieces, then adds 100mL ethanol, and leave standstill 24h.Finally by with the gel filtered in drying machine, at 60 DEG C, dry 10h, grinds product with mortar, is preserved by powder-tight, lucifuge, to be Protected from Heat.
2) preparation of the long-acting type intelligence inhibiter of pH Co ntrolled release
Be in the aqueous solution of 8 by the dry gel powder of above-mentioned for the 0.1g gained pH be dissolved in containing benzotriazole (BTA) inhibiter, BTA concentration is 5mg/mL, leave standstill 48 hours, gained is carried inhibiter hydrogel washed with de-ionized water three times, after vacuum lyophilization, grind into powder sealing preserve, for subsequent use.
Embodiment 4
1) preparation of the hydrogel of pH sensitivity
A) joining in the there-necked flask with prolong, agitator and thermometer by 2.0g starch, adding 35mL distilled water, passing into nitrogen, stirring velocity is 300 revs/min, is warming up to 80 DEG C gradually.0.1g ammonium persulfate initiator is dissolved in 5mL deionized water, is joining in above-mentioned reactant aqueous solution, maintaining nitrogen purge, stable reaction 10min.1.5g vinylformic acid and 1.5g hydroxyethyl methylacrylate are joined in above-mentioned reactant aqueous solution; 0.05g methylene-bisacrylamide linking agent is same as in 5mL deionized water, joins in above-mentioned reactant aqueous solution, control to react 60min under above-mentioned stirring velocity and temperature.
B), after reaction terminates, room temperature is cooled to, and with the NaOH solution adjust pH to 8 of 1M.Add 0.05g sodium bicarbonate whipping agent, stirring velocity is 500 revs/min, to producing uniform form of foam.The hydrogel of gained is injected excessive ethanol, leaves standstill 3h; By ethanol everywhere, and product is cut into small pieces, then adds 100mL ethanol, and leave standstill 24h.Finally by with the gel filtered in drying machine, at 60 DEG C, dry 10h, grinds product with mortar, is preserved by powder-tight, lucifuge, to be Protected from Heat.
2) preparation of the long-acting type intelligence inhibiter of pH Co ntrolled release
Be in the aqueous solution of 8 by the dry gel powder of above-mentioned for the 0.1g gained pH be dissolved in containing imidazoline inhibitor, tetrahydroglyoxaline concentration is 5mg/mL, leaves standstill 48 hours, gained is carried inhibiter hydrogel washed with de-ionized water three times, after vacuum lyophilization, grind into powder sealing preserve, for subsequent use.
Embodiment 5
1) preparation of the hydrogel of pH sensitivity
A) joining in the there-necked flask with prolong, agitator and thermometer by 2.0g starch, adding 35mL distilled water, passing into nitrogen, stirring velocity is 300 revs/min, is warming up to 80 DEG C gradually.0.1g ammonium persulfate initiator is dissolved in 5mL deionized water, is joining in above-mentioned reactant aqueous solution, maintaining nitrogen purge, stable reaction 10min.1.5g vinylformic acid and 1.5g hydroxyethyl methylacrylate are joined in above-mentioned reactant aqueous solution; 0.05g methylene-bisacrylamide linking agent is same as in 5mL deionized water, joins in above-mentioned reactant aqueous solution, control to react 60min under above-mentioned stirring velocity and temperature.
B), after reaction terminates, room temperature is cooled to, and with the NaOH solution adjust pH to 8 of 1M.Add 0.05g sodium bicarbonate whipping agent, stirring velocity is 500 revs/min, to producing uniform form of foam.The hydrogel of gained is injected excessive ethanol, leaves standstill 3h; By ethanol everywhere, and product is cut into small pieces, then adds 100mL ethanol, and leave standstill 24h.Finally by with the gel filtered in drying machine, at 60 DEG C, dry 10h, grinds product with mortar, is preserved by powder-tight, lucifuge, to be Protected from Heat.
2) preparation of the long-acting type intelligence inhibiter of pH Co ntrolled release
Be in the aqueous solution of 8 by the dry gel powder of above-mentioned for the 0.1g gained pH be dissolved in containing imidazolidine derivatives inhibiter, imidazolidine derivatives concentration is 5mg/mL, leave standstill 48 hours, gained is carried inhibiter hydrogel washed with de-ionized water three times, after vacuum lyophilization, grind into powder sealing preserve, for subsequent use.
Claims (2)
1. one kind can by the preparation method of the long-acting intelligent inhibiter of pH Co ntrolled release, it is characterized in that: be 5%-10% by the macromolecular material content with three-dimensional network, monomer content is 5%-10%, initiator content is 0.01-0.1 times of monomer, content of crosslinking agent is 0.01-0.1 times of monomer mass, Content of Pore-forming Agents is 0.05%-0.15%, inhibiter content is 5-15mg/mL composition, the described macromolecular material with three-dimensional network is one of starch or chitosan, described monomer is vinylformic acid, one of methacrylic acid or hydroxyethyl methylacrylate, described linking agent is one of methylene-bisacrylamide or four condensed ethandiol double methacrylates, described initiator is one of ammonium persulphate or Potassium Persulphate, described pore-forming material is one of sodium bicarbonate or acetone, its preparation method includes following steps:
1) preparation of the hydrogel of pH response
A the macromolecular material with three-dimensional network is placed in the there-necked flask with prolong, agitator and thermometer by (), the deionized water adding 20-40mL is mixed with the aqueous solution, pass into nitrogen and Keep agitation, stirring velocity is 200-500 rev/min, keep being warming up to 60-100 DEG C, then in aqueous solutions of polymers, add initiator, reaction for some time after add monomer and linking agent, and under 60-100 DEG C of constant temperature sustained reaction 60-180min;
B () reaction terminates after, be cooled to room temperature, and regulate pH with one of NaOH aqueous solution of HCl or 1M of 1M, add pore-forming material, and uniform stirring; Products therefrom is poured in ethanol and cleans, after leaving standstill 3-5h, ethanol is poured out, product is put into loft drier dry, obtain xerogel;
2) preparation of the long-acting intelligent inhibiter of pH Co ntrolled release
Described xerogel is dissolved in the aqueous solution containing inhibiter, soaks 2-4 days, filter, and through vacuum lyophilization, namely obtaining can by the long-acting intelligent inhibiter of pH Co ntrolled release.
2. according to claim 1ly a kind ofly by the preparation method of the long-acting intelligent inhibiter of pH Co ntrolled release, can to it is characterized in that, described inhibiter is benzotriazole.
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| CN104725563B (en) * | 2013-12-19 | 2017-04-12 | 中国科学院金属研究所 | Corrosion inhibitor gel microsphere with intelligent pH value controlled release function and its preparation method and use |
| CN104593779B (en) * | 2015-01-21 | 2018-02-16 | 北京科技大学 | A kind of preparation method of the intelligent corrosion inhibiter of low pH controlled releases |
| CN105668813B (en) * | 2016-01-25 | 2019-04-26 | 苏州他山石环保科技有限公司 | A kind of antisludging agent and preparation method thereof |
| CN106868512B (en) * | 2016-12-22 | 2019-03-19 | 德蓝水技术股份有限公司 | A kind of high temperature resistant acidification corrosion inhibitor and preparation method thereof |
| CN107226987A (en) * | 2017-07-13 | 2017-10-03 | 怀宁县牧之金畜禽实业有限责任公司 | A kind of preparation method of biomass grafted chitosan anti-biotic material |
| CN108070864B (en) * | 2017-12-25 | 2020-11-24 | 重庆工业职业技术学院 | pH value response intelligent control release corrosion inhibitor and preparation method thereof |
| CN109021629A (en) * | 2018-07-12 | 2018-12-18 | 中国科学院海洋研究所 | A kind of environmentally friendly selfreparing hydrogel anticorrosive paint and its synthetic method |
| CN108914190B (en) * | 2018-08-03 | 2020-03-31 | 中国科学院金属研究所 | Preparation method of magnesium alloy surface micro-arc oxidation/intelligent slow-release structure integrated composite coating |
| CN111592121B (en) * | 2020-05-13 | 2021-10-08 | 欣格瑞（山东）环境科技有限公司 | Acrylic copolymer, corrosion and scale inhibitor composition and application |
| CN115057957B (en) * | 2022-08-18 | 2022-11-04 | 山东诺尔生物科技有限公司 | Preparation method of super water-absorbing material and super water-absorbing material |
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