CN105951104A - Preparation method of environment-friendly metal corrosion inhibitor - Google Patents
Preparation method of environment-friendly metal corrosion inhibitor Download PDFInfo
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- CN105951104A CN105951104A CN201610547461.XA CN201610547461A CN105951104A CN 105951104 A CN105951104 A CN 105951104A CN 201610547461 A CN201610547461 A CN 201610547461A CN 105951104 A CN105951104 A CN 105951104A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/144—Aminocarboxylic acids
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a preparation method of an environment-friendly metal corrosion inhibitor, and belongs to the technical field of preparation of corrosion inhibitors. Polygala tenuifolia root particles and anhydrous ethanol are mixed, heated and filtered; then, filtrate is collected; the filtrate and sodium hydroxide are mixed and heated, and are added with hydrochloric acid solution for reaction; then, mixed solution is collected to evaporate to prepare dry polygala tenuifolia saponin crystals; beta-alanine, sodium hydroxide, de-ionized water and anhydrous ethanol are mixed to prepare amino acid modified liquid; then, the dry polygala tenuifolia saponin crystals and sodium hydroxide are mixed and heated to prepare polygala tenuifolia saponin mixed liquid; the polygala tenuifolia saponin mixed liquid and the amino acid modified liquid are mixed and heated, and are added with the hydrochloric acid solution for reaction; and prepared dry filter cakes and anhydrous ethanol are mixed, heated, stood and aged to obtain the environment-friendly metal corrosion inhibitor. Proved by examples, the preparation method is convenient for operation, adds no poisonous substances, is safe and healthy, cannot cause harm to humans and environments, and cannot cause new corrosion problems.
Description
Technical field
The invention discloses the preparation method of a kind of environment-friendly metal corrosion inhibiter, belong to corrosion inhibiter preparing technical field.
Background technology
Metal erosion refers to the destruction or rotten that metal causes under the effect of external environment.During corrosion, the interface of metal there occurs chemistry or electrochemistry heterogeneous reaction, make metal proceed to aoxidize (ion) state.This can significantly reduce the mechanical properties such as the intensity of metal material, plasticity, toughness, destroy the geometry of hardware, increase the abrasion between part, deteriorate the physical properties such as electrical and optical, in the service life of shortening equipment, even cause the catastrophic failure such as fire, blast.Corrosion not only have impact on the gloss of original metal, and brings the biggest economic loss.
Adding certain material minimal amount of in corrosive environment, metal erosion speed can be made to be substantially reduced, this material is just corrosion inhibiter, is also corrosion inhibitor.Corrosion inhibiter can be single-component substance, or multicomponent feature is: easy to use, small investment, protected effect are good, consumption is the least, but effect is notable.
Corrosion inhibiter is a kind of inorganic matter or Organic substance, is added in corrosive medium, by means of this material physics on the interface of metal and corrosive medium and chemical action, is possible to prevent or reduces corrosion of metal speed, reduce metal corrosion in media as well.Corrosion inhibiter application in metal protection, is a serious achievement of corrosion science and the development of Surface Engineering subject.Century-old remaining come, the exploitation of corrosion inhibiter, apply in the fields such as chemical industry, oil, electric power, machinery, intermetallic composite coating, transportation, nuclear energy and space flight, play an important role.The most in half a century, the kind of corrosion inhibiter, quality have obtained further expansion and raising.
Inhibition efficiency is bigger, and the effect of suppression corrosion is better.Sometimes several inhomogeneity corrosion inhibiter of relatively low-dose can obtain preferable corrosion mitigating effect by formula compound use, improves inhibition efficiency, and this effect is referred to as cooperative effect;If on the contrary, reducing respective inhibition efficiency, the most referred to as negative coopertive effect, also referred to as antagonistic effect when dissimilar corrosion inhibiter is used in conjunction with on the contrary.
Metal current corrosion inhibiter the most all contains noxious substance, easily works the mischief human body and environment, and in use improper use, easily causes new etching problem.
Summary of the invention
The technical problem that present invention mainly solves: for current existing metal inhibitor containing noxious substance, easily human body and environment are worked the mischief, and in use improper use, the problem easily causing new corrosion, the preparation method of a kind of environment-friendly metal corrosion inhibiter is provided, the method is by payta granule and dehydrated alcohol mixing heating, filtrate is then collected by filtration, then by filtrate and sodium hydroxide Hybrid Heating and add hydrochloric acid solution and react, then collect mixed solution evaporation and prepare dry polygalic acid crystallization, by Beta-alanine, sodium hydroxide, deionized water and dehydrated alcohol are mixed with to obtain amino-acid modified liquid；Then the crystallization of dry polygalic acid is mixed with sodium hydroxide, heating is prepared into polygalic acid mixed liquor, subsequently polygalic acid mixed liquor is mixed and heated with amino-acid modified liquid and adds hydrochloric acid solution and react, the dry cake that will prepare, with dehydrated alcohol Hybrid Heating, still aging, a kind of environment-friendly metal corrosion inhibiter；The method extracts polygalic acid by payta, is chelated mutually with metal by polygalic acid, forms coat of metal, effectively prepares green metal corrosion inhibiter safety and Health, will not work the mischief human body and environment, and not result in new etching problem.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) dry payta is chosen, shredded and milled and sieved, it is prepared into 75～80 mesh payta granules, 1:10 in mass ratio, payta granule is mixed with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, wait refluxing after 2～3h, standing is cooled to room temperature, filters and collects filtrate；
(2) 1:5 in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 1～2h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 65～80 DEG C, collect and be dried polygalic acid crystallization, standby；
(3) count by weight, weigh 25～30 parts of Beta-alanines, 10～15 parts of sodium hydroxide, 45～50 parts of deionized waters and 35～40 parts of dehydrated alcohol respectively to be placed in there-necked flask, stirring mixing is placed in ice bath mixing 10～15min at 0～5 DEG C, is prepared into amino-acid modified liquid；
(4) 1:5 in mass ratio, dry polygalic acid crystallization step (2) prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 10～15min at 45～50 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 1～2h at 65～80 DEG C；
(5) after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 65～80 DEG C, it is dried 6～8h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, it is placed in heating in water bath 1～2h at 65～80 DEG C, the most still aging 20～24h, a kind of environment-friendly metal corrosion inhibiter can be prepared into.
The using method of the present invention is: the environment-friendly metal corrosion inhibiter present invention prepared adds the metal embathed or containing in the metal of corrosive medium; addition is the 0.1～0.5% of total metal mass; after testing; the metal inhibitor corrosion mitigating effect using the present invention to prepare is preferable; corrosion inhibition rate reaches more than 95%, has preferable protective effect to metal.
The invention has the beneficial effects as follows:
(1) present invention does not contains noxious substance, natural safety and environmental protection, to human body and environment non-hazardous, and will not produce new etching problem；
(2) raw material of the present invention is easy to get, and the gentle preparation process of reaction is simple, effectively save preparation time and cost.
Detailed description of the invention
First dry payta is chosen, shredded and milled and sieved, it is prepared into 75～80 mesh payta granules, 1:10 in mass ratio, payta granule is mixed with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, wait refluxing after 2～3h, standing is cooled to room temperature, filters and collects filtrate；1:5 the most in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 1～2h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 65～80 DEG C, collect and be dried polygalic acid crystallization, standby；Count the most by weight, weigh 25～30 parts of Beta-alanines, 10～15 parts of sodium hydroxide, 45～50 parts of deionized waters and 35～40 parts of dehydrated alcohol respectively to be placed in there-necked flask, stirring mixing is placed in ice bath mixing 10～15min at 0～5 DEG C, is prepared into amino-acid modified liquid；1:5 the most in mass ratio, dry polygalic acid crystallization above-mentioned steps prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 10～15min at 45～50 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 1～2h at 65～80 DEG C；Finally after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 65～80 DEG C, it is dried 6～8h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, be placed in heating in water bath 1～2h at 65～80 DEG C, the most still aging 20～24h, a kind of environment-friendly metal corrosion inhibiter.
Example 1
First choose dry payta, shredded and mill and sieve, be prepared into 75 mesh payta granules, 1:10 in mass ratio, mixes payta granule with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, after backflow 2h, stand and be cooled to room temperature, filter and collect filtrate；1:5 the most in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 1h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 65 DEG C, collect and be dried polygalic acid crystallization, standby；Counting the most by weight, weigh 25 parts of Beta-alanines, 10 parts of sodium hydroxide, 45 parts of deionized waters and 35 parts of dehydrated alcohol respectively and be placed in there-necked flask, stirring mixing is placed in ice bath mixing 10min at 0 DEG C, is prepared into amino-acid modified liquid；1:5 the most in mass ratio, dry polygalic acid crystallization above-mentioned steps prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 10min at 45 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 1h at 65 DEG C；Finally after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 65 DEG C, it is dried 6h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, be placed in heating in water bath 1h at 65 DEG C, the most still aging 20h, a kind of environment-friendly metal corrosion inhibiter.
This example operation is easy; during use; the environment-friendly metal corrosion inhibiter present invention prepared adds the metal embathed or containing in the metal of corrosive medium; addition is 0.1%; after testing; the metal inhibitor corrosion mitigating effect using the present invention to prepare is preferable, and corrosion inhibition rate reaches 95%, has preferable protective effect to metal.
Example 2
First choose dry payta, shredded and mill and sieve, be prepared into 78 mesh payta granules, 1:10 in mass ratio, mixes payta granule with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, after backflow 2.5h, stand and be cooled to room temperature, filter and collect filtrate；1:5 the most in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 1.5h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 73 DEG C, collect and be dried polygalic acid crystallization, standby；Counting the most by weight, weigh 28 parts of Beta-alanines, 13 parts of sodium hydroxide, 48 parts of deionized waters and 38 parts of dehydrated alcohol respectively and be placed in there-necked flask, stirring mixing is placed in ice bath mixing 13min at 3 DEG C, is prepared into amino-acid modified liquid；1:5 the most in mass ratio, dry polygalic acid crystallization above-mentioned steps prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 13min at 48 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 1.5h at 73 DEG C；Finally after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 73 DEG C, it is dried 7h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, be placed in heating in water bath 1.5h at 73 DEG C, the most still aging 22h, a kind of environment-friendly metal corrosion inhibiter.
This example operation is easy; during use; the environment-friendly metal corrosion inhibiter present invention prepared adds the metal embathed or containing in the metal of corrosive medium; addition is 0.3%; after testing; the metal inhibitor corrosion mitigating effect using the present invention to prepare is preferable, and corrosion inhibition rate reaches 97%, has preferable protective effect to metal.
Example 3
First choose dry payta, shredded and mill and sieve, be prepared into 80 mesh payta granules, 1:10 in mass ratio, mixes payta granule with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, after backflow 3h, stand and be cooled to room temperature, filter and collect filtrate；1:5 the most in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 2h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 80 DEG C, collect and be dried polygalic acid crystallization, standby；Counting the most by weight, weigh 30 parts of Beta-alanines, 15 parts of sodium hydroxide, 50 parts of deionized waters and 40 parts of dehydrated alcohol respectively and be placed in there-necked flask, stirring mixing is placed in ice bath mixing 15min at 5 DEG C, is prepared into amino-acid modified liquid；1:5 the most in mass ratio, dry polygalic acid crystallization above-mentioned steps prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 15min at 50 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 2h at 80 DEG C；Finally after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 80 DEG C, it is dried 8h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, be placed in heating in water bath 2h at 80 DEG C, the most still aging 24h, a kind of environment-friendly metal corrosion inhibiter.
This example operation is easy; during use; the environment-friendly metal corrosion inhibiter present invention prepared adds the metal embathed or containing in the metal of corrosive medium; addition is 0.1%; after testing; the metal inhibitor corrosion mitigating effect using the present invention to prepare is preferable, and corrosion inhibition rate reaches 99%, has preferable protective effect to metal.
Claims (1)
1. the preparation method of an environment-friendly metal corrosion inhibiter, it is characterised in that concrete preparation process is:
(1) dry payta is chosen, shredded and milled and sieved, it is prepared into 75～80 mesh payta granules, 1:10 in mass ratio, payta granule is mixed with absolute ethyl alcohol and stirring and is placed in conical flask, be subsequently heated to backflow, wait refluxing after 2～3h, standing is cooled to room temperature, filters and collects filtrate；
(2) 1:5 in mass ratio, the filtrate of above-mentioned collection is mixed with the stirring of mass concentration 10% sodium hydroxide and is placed in conical flask, after being heated to reflux 1～2h, conical flask is dripped mass concentration 10% hydrochloric acid solution, after dropping to pH and being 7.0, collect mixed solution and be placed in rotary evaporated to dryness at 65～80 DEG C, collect and be dried polygalic acid crystallization, standby；
(3) count by weight, weigh 25～30 parts of Beta-alanines, 10～15 parts of sodium hydroxide, 45～50 parts of deionized waters and 35～40 parts of dehydrated alcohol respectively to be placed in there-necked flask, stirring mixing is placed in ice bath mixing 10～15min at 0～5 DEG C, is prepared into amino-acid modified liquid；
(4) 1:5 in mass ratio, dry polygalic acid crystallization step (2) prepared mixes with the stirring of 1mol/L sodium hydroxide, heating in water bath 10～15min at 45～50 DEG C, it is prepared into polygalic acid mixed liquor, 1:2 the most in mass ratio, stir to mix with the amino-acid modified liquid of above-mentioned preparation by polygalic acid mixed liquor and be placed in there-necked flask, heating in water bath 1～2h at 65～80 DEG C；
(5) after heating in water bath completes, there-necked flask is dripped mass concentration 15% hydrochloric acid solution, and after dropping to there-necked flask and producing without precipitation, sucking filtration also collects filter cake, and be washed with deionized to pH to 7.0, at 65～80 DEG C, it is dried 6～8h again, is prepared into dry cake, the most in mass ratio 1:10, dry cake is mixed with absolute ethyl alcohol and stirring, it is placed in heating in water bath 1～2h at 65～80 DEG C, the most still aging 20～24h, a kind of environment-friendly metal corrosion inhibiter can be prepared into.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610547461.XA CN105951104A (en) | 2016-07-13 | 2016-07-13 | Preparation method of environment-friendly metal corrosion inhibitor |
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| CN201610547461.XA CN105951104A (en) | 2016-07-13 | 2016-07-13 | Preparation method of environment-friendly metal corrosion inhibitor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108425119A (en) * | 2018-04-09 | 2018-08-21 | 翟琳 | A kind of preparation method of metal inhibitor |
| CN109576688A (en) * | 2019-02-01 | 2019-04-05 | 浙江外国语学院 | Chemical nickel-plating solution, nickel plating process and the nickel plating part of the hydrolyzate containing sapindoside |
| CN117702125A (en) * | 2023-11-08 | 2024-03-15 | 宁波维创柔性电子技术有限公司 | Preparation method of rust-proof master batch composite vapor phase corrosion inhibitor for rust-proof film |
-
2016
- 2016-07-13 CN CN201610547461.XA patent/CN105951104A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108425119A (en) * | 2018-04-09 | 2018-08-21 | 翟琳 | A kind of preparation method of metal inhibitor |
| CN109576688A (en) * | 2019-02-01 | 2019-04-05 | 浙江外国语学院 | Chemical nickel-plating solution, nickel plating process and the nickel plating part of the hydrolyzate containing sapindoside |
| CN117702125A (en) * | 2023-11-08 | 2024-03-15 | 宁波维创柔性电子技术有限公司 | Preparation method of rust-proof master batch composite vapor phase corrosion inhibitor for rust-proof film |
| CN117702125B (en) * | 2023-11-08 | 2024-05-28 | 宜兴维新科技有限公司 | Preparation method of rust-proof master batch composite vapor phase corrosion inhibitor for rust-proof film |
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Application publication date: 20160921 |