CN104213124A - Method for manufacturing water-based metal antirust agents - Google Patents
Method for manufacturing water-based metal antirust agents Download PDFInfo
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- CN104213124A CN104213124A CN201410446188.2A CN201410446188A CN104213124A CN 104213124 A CN104213124 A CN 104213124A CN 201410446188 A CN201410446188 A CN 201410446188A CN 104213124 A CN104213124 A CN 104213124A
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Abstract
The invention relates to the technical field of metal rust protection, in particular to a method for manufacturing water-based metal antirust agents. The method comprises the following steps that caprolactam and sodium hydroxide are put into water according to the molar ratio of 1:0.8 to 1.5, temperature rises to 60 DEG C to 100 DEG C, and the temperature is kept for three hours to ten hours; (2) the temperature is cooled to 0 DEG C to 20 DEG C, and 1/5 to 1/3 of the molar weight of caprolactam is put according to the step (1), cyanuric chloride is added, heat preservation is carried out for one to three hours, sodium hydroxide is added, and the PH value is adjusted to 7.5 to 12; (3) temperature rises to 70 DEG C to 100 DEG C, the temperature is kept for five hours, and the sodium hydroxide is used for adjusting the PH value to 7.5 to 12; (4) the temperature is cooled to 30 DEG C to 50 DEG C, solutions are filtered, then, hydrochloric acid is added to enable the PH value to one to three, circulating stirring is carried out, and the heat preservation is carried out for one to five hours at the temperature of 30 DEG C to 60 DEG C. The method for manufacturing the water-based metal antirust agents has the advantages of being environmentally friendly, high in yield, high in product purity, excellent in product performance and low in cost.
Description
Technical field
The present invention relates to metal antirusting technical field, be specifically related to a kind of preparation method of water metal rust-resisting agent.
Background technology
The every profession and trades such as metal widespread use and machinery, automobile, household electrical appliances, building.Metal rusting affects equipment performance, even needs to scrap process.In order to improve metallicity, reducing corrosion waste, needing its surperficial antirust treatment.
Water-based antirust agent has the advantages such as safe, easy to operate, with low cost.The water-based antirust agent of current use is mainly with nitrite for main component is formulated, and nitrite water-based antirust agent is widely used.But nitrite is carcinogenic substance, there is larger toxicity, have larger harm to human body and environment.
Prior art does not contain the organic water borne rust-preventive agent of nitrite from a manufacturer---and Ciba (Ciba Specialty Chemicals), its L190 water-based antirust agent has good performance.But the synthetic technology of Ciba is secret.
Summary of the invention
The present invention obtains a kind of preparation method of water metal rust-resisting agent through experiment, has environmental protection, yield is high, product purity is high, product performance are superior, becomes local advantage.
The preparation method of a kind of water metal rust-resisting agent of the present invention, comprises the following steps:
(1), by hexanolactam and sodium hydroxide drop in water 1:0.8 ~ 1.5 in molar ratio, make water account for 70 ~ 90% of total mass; Be warming up to 60 ~ 100 DEG C and keep 3 ~ 10 hours;
(2), by the solution that step (1) obtains cool to 0 ~ 20 DEG C, drop into 1/5 ~ 1/3 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 1 ~ 3 hour, add sodium hydroxide and regulate pH value to 7.5 ~ 12;
(3), be warming up to 70 ~ 100 DEG C and keep 5 hours, regulating pH value to 7.5 ~ 12 with sodium hydroxide;
(4), be cooled to 20 ~ 50 DEG C, add hydrochloric acid after filtration and make pH value be 1 ~ 3; 30 ~ 60 DEG C of insulations 1 ~ 5 hour after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.Deionized water wash, refers to eliminating the pure water after in ionic species impurity.
Preferably, hexanolactam and sodium hydroxide drop in water 1:0.8 ~ 1 by described step (1) in molar ratio, make water account for 70 ~ 90% of total mass; Be warming up to 70 ~ 100 DEG C and keep 3 ~ 10 hours.
In the preparation method of a kind of water metal rust-resisting agent of the present invention, the temperature of each composition and proportioning, each step and hold-time are all the key parameters of preparation, obtained, can ensure that chemical reaction fully carries out by experiment.Especially in step (2) and step (3), twice practical sodium hydroxide regulates pH value, guarantees sufficient reacting, such that product yield is high, impurity is few.The preparation method inventing a kind of water metal rust-resisting agent produces the yield of rust-preventive agent can up to more than 80%.
The rust-preventive agent major ingredient that the preparation method of a kind of water metal rust-resisting agent of the present invention obtains is ternary poly carboxylic acid, acid number is 100 ~ 700mgKOH/g, chloride ion content is 100 ~ 500ppm, has outstanding rustless property, can substitute the vapour bar L190 water-based antirust agent of currently available products.
Embodiment
Below the preferred embodiment of the present invention is further described.The composition combination stated in summary of the invention and quality all belong to protection scope of the present invention than scope, and embodiment is not considered as limiting the scope of the invention.
Embodiment one:
The preparation method of a kind of water metal rust-resisting agent of the present invention, comprises the following steps:
(1), by hexanolactam and sodium hydroxide in molar ratio 1:1 drop in water, make water account for 80% of total mass; Be warming up to 80 DEG C and keep 6 hours;
(2), by the solution that step (1) obtains cool to 10 DEG C, drop into 1/4 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 2 hours, add sodium hydroxide and regulate pH value to 9;
(3), be warming up to 80 DEG C and keep 5 hours, regulating pH value to 9 with sodium hydroxide;
(4), be cooled to 40 DEG C, add hydrochloric acid after filtration and make pH value be 2; 40 DEG C of insulations 3 hours after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.
Embodiment two:
The preparation method of a kind of water metal rust-resisting agent of the present invention, comprises the following steps:
(1), by hexanolactam and sodium hydroxide in molar ratio 1:0.9 drop in water, make water account for 70% of total mass; Be warming up to 60 DEG C and keep 10 hours;
(2), by the solution that step (1) obtains cool to 5 DEG C, drop into 1/5 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 3 hours, add sodium hydroxide and regulate pH value to 7.5;
(3), be warming up to 70 DEG C and keep 5 hours, regulating pH value to 7.5 with sodium hydroxide;
(4), be cooled to 30 DEG C, add hydrochloric acid after filtration and make pH value be 1; 30 DEG C of insulations 5 hours after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.
Embodiment three:
The preparation method of a kind of water metal rust-resisting agent of the present invention, comprises the following steps:
(1), by hexanolactam and sodium hydroxide in molar ratio 1:1.5 drop in water, make water account for 90% of total mass; Be warming up to 60 DEG C and keep 3 hours;
(2), by the solution that step (1) obtains cool to 20 DEG C, drop into 1/3 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 3 hours, add sodium hydroxide and regulate pH value to 10;
(3), be warming up to 100 DEG C and keep 5 hours, regulating pH value to 10 with sodium hydroxide;
(4), be cooled to 30 DEG C, add hydrochloric acid after filtration and make pH value be 3; 30 DEG C of insulations 5 hours after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.
Embodiment four:
The preparation method of a kind of water metal rust-resisting agent of the present invention, comprises the following steps:
(1), by hexanolactam and sodium hydroxide in molar ratio 1:1.2 drop in water, make water account for 85% of total mass; Be warming up to 90 DEG C and keep 7 hours;
(2), by the solution that step (1) obtains cool to 15 DEG C, drop into 1/3 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 1.5 hours, add sodium hydroxide and regulate pH value to 10;
(3), be warming up to 90 DEG C and keep 5 hours, regulating pH value to 10 with sodium hydroxide;
(4), be cooled to 45 DEG C, add hydrochloric acid after filtration and make pH value be 1; 45 DEG C of insulations 4 hours after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.
Claims (2)
1. a preparation method for water metal rust-resisting agent, is characterized in that: comprise the following steps:
(1), by hexanolactam and sodium hydroxide drop in water 1:0.8 ~ 1.5 in molar ratio, make water account for 70 ~ 90% of total mass; Be warming up to 60 ~ 100 DEG C and keep 3 ~ 10 hours;
(2), cool to 0 ~ 20 DEG C, drop into 1/5 ~ 1/3 of hexanolactam molar weight by step (1) and add cyanuric chloride; Be incubated after 1 ~ 3 hour, add sodium hydroxide and regulate pH value to 7.5 ~ 12;
(3), be warming up to 70 ~ 100 DEG C and keep 5 hours, regulating pH value to 7.5 ~ 12 with sodium hydroxide;
(4), be cooled to 20 ~ 50 DEG C, add hydrochloric acid after filtration and make pH value be 1 ~ 3; 30 ~ 60 DEG C of insulations 1 ~ 5 hour after circulation stirring;
(5), press filtration obtains solid;
(6), by after solid deionized water wash again press filtration obtain product.
2. the preparation method of a kind of water metal rust-resisting agent as claimed in claim 1, is characterized in that: hexanolactam and sodium hydroxide drop in water 1:0.8 ~ 1 by described step (1) in molar ratio, make water account for 70 ~ 90% of total mass; Be warming up to 70 ~ 100 DEG C and keep 3 ~ 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410446188.2A CN104213124A (en) | 2014-09-04 | 2014-09-04 | Method for manufacturing water-based metal antirust agents |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410446188.2A CN104213124A (en) | 2014-09-04 | 2014-09-04 | Method for manufacturing water-based metal antirust agents |
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| CN104213124A true CN104213124A (en) | 2014-12-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818077A (en) * | 2015-03-11 | 2015-08-05 | 洛阳绿帆功能化学有限公司 | Water-based antirust multifunctional additive with high hard water resistance, preparation method and application thereof |
| CN108102354A (en) * | 2017-12-29 | 2018-06-01 | 中南大学 | A kind of well lid anticorrosion material and preparation method thereof |
| CN109836707A (en) * | 2018-10-30 | 2019-06-04 | 广州芬豪香精有限公司 | A kind of preparation method of chemical raw material case |
| CN110592594A (en) * | 2019-10-16 | 2019-12-20 | 洛阳太平洋联合石油化工有限公司 | Quaternary carboxylic acid metal antirust agent and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4402907A (en) * | 1980-08-13 | 1983-09-06 | Ciba-Geigy Corporation | Triazine carboxylic acids as corrosion inhibitors for aqueous systems |
| DE10208591A1 (en) * | 2002-02-27 | 2003-11-20 | Degussa | Crystallization of melamine tris-alkanoic acid for use, e.g., as corrosion inhibitor involves precipitation from alkaline aqueous solution by adding acid at elevated temperature |
| CN101973949A (en) * | 2010-11-17 | 2011-02-16 | 天津师范大学 | Method for preparing 2,4,6-tri(amino caproyl)-1,3,5-triazine |
| CN102659700A (en) * | 2012-03-05 | 2012-09-12 | 浙江金科过氧化物股份有限公司 | Production process of granular 2,4,6-tri(amino caproyl)-1,3,5-triazine having low chlorine content |
-
2014
- 2014-09-04 CN CN201410446188.2A patent/CN104213124A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4402907A (en) * | 1980-08-13 | 1983-09-06 | Ciba-Geigy Corporation | Triazine carboxylic acids as corrosion inhibitors for aqueous systems |
| DE10208591A1 (en) * | 2002-02-27 | 2003-11-20 | Degussa | Crystallization of melamine tris-alkanoic acid for use, e.g., as corrosion inhibitor involves precipitation from alkaline aqueous solution by adding acid at elevated temperature |
| CN101973949A (en) * | 2010-11-17 | 2011-02-16 | 天津师范大学 | Method for preparing 2,4,6-tri(amino caproyl)-1,3,5-triazine |
| CN102659700A (en) * | 2012-03-05 | 2012-09-12 | 浙江金科过氧化物股份有限公司 | Production process of granular 2,4,6-tri(amino caproyl)-1,3,5-triazine having low chlorine content |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818077A (en) * | 2015-03-11 | 2015-08-05 | 洛阳绿帆功能化学有限公司 | Water-based antirust multifunctional additive with high hard water resistance, preparation method and application thereof |
| CN104818077B (en) * | 2015-03-11 | 2017-03-29 | 洛阳理工学院 | A kind of aqueous rustproof multifunction additive of anti-high hardness and its production and use |
| CN108102354A (en) * | 2017-12-29 | 2018-06-01 | 中南大学 | A kind of well lid anticorrosion material and preparation method thereof |
| CN109836707A (en) * | 2018-10-30 | 2019-06-04 | 广州芬豪香精有限公司 | A kind of preparation method of chemical raw material case |
| CN110592594A (en) * | 2019-10-16 | 2019-12-20 | 洛阳太平洋联合石油化工有限公司 | Quaternary carboxylic acid metal antirust agent and preparation method and application thereof |
| CN110592594B (en) * | 2019-10-16 | 2021-08-17 | 洛阳太平洋联合石油化工有限公司 | Quaternary carboxylic acid metal antirust agent and preparation method and application thereof |
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Application publication date: 20141217 |