CN102296297B - Aqueous metal anti-rust agent - Google Patents
Aqueous metal anti-rust agent Download PDFInfo
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- CN102296297B CN102296297B CN201110230921A CN201110230921A CN102296297B CN 102296297 B CN102296297 B CN 102296297B CN 201110230921 A CN201110230921 A CN 201110230921A CN 201110230921 A CN201110230921 A CN 201110230921A CN 102296297 B CN102296297 B CN 102296297B
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- water
- hexahydroaniline
- antirust agent
- based antirust
- citrate trianion
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- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses an aqueous metal anti-rust agent containing cyclohexylamine citrate. The aqueous metal anti-rust agent has good anti-rust effects on iron, steel, iron alloys, aluminum, copper and the like, and thus can be utilized for rust protection of metal equipment and parts, wherein the metal equipment and parts are made of iron, steel, iron alloys, aluminum, copper and the like.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of metal antirusting agent that contains the water-based of hexahydroaniline Citrate trianion.
Background technology
At present, widely-used water-based antirust agent in metal rust preventing.Water-based antirust agent has safety, improve and simplify production technique, advantage such as reduce production costs.Yet the water-based antirust agent that uses at present is how formulated as staple with nitrite.Nitrite is the carinogenicity material, has big toxicity, and people, animal, environment etc. are had bigger harm.Therefore the water-based antirust agent that does not contain nitrite is developed in expectation.
For example the open CN101532131 of Chinese patent discloses a kind of long-acting water-based metal rust inhibitor, and it contains phytic acid, thanomin, borax class and acid amides.This rust-preventive agent it is said nontoxic, harmless, free from environmental pollution.
In addition, the open CN101565582A of Chinese patent discloses a kind of metal antirusting agent, and it contains sorbyl alcohol, trolamine, phenylformic acid, boric acid, POTASSIUM SORBATE GRANULAR WHITE, glycerine, horse propylene copolymer, sodium hydroxide, yellow soda ash.This rust-preventive agent does not contain heavy metal and carcinogenic substance Sodium Nitrite, can not damage human body.
In addition, the open CN102010626A of Chinese patent discloses a kind of environment-friendly water-based rust-preventive agent, and it contains boric acid, thanomin, neutralizing agent, inhibiter, additive and water.This rust-preventive agent does not contain that nitrite, phosphoric acid salt, dichromate etc. are poisonous, objectionable impurities, non-stimulated to human body, do not have an injury.
Existing at present employing hexahydroaniline and/or its inorganic acid salt are as the sanitas in the water-based antirust agent.CN 1140189A discloses the water-based antirust agent that contains polyglycol and nitrite cyclohexylamine etc.CN1754986A discloses the metal surface passivant that contains hexahydroaniline and tsp.CN101298678A discloses metal antirusting agent, and it contains hexahydroaniline 10～15%, laurostearic acid 15～20%, cyclohexylamine carbonate 5～9%, benzotriazole 0.2～0.4%, surplus is water.Yet these use the inorganic acid salt of hexahydroaniline, and are still undesirable on antiseptic property.
Yet the rust-preventive agent of more than mentioning still remains to be improved at aspects such as rustless property, preparation convenience, production costs.Still exist demand for further improvement of rustless property and the good novel aqueous rust-preventive agent of the feature of environmental protection.
Summary of the invention
The metal antirusting agent that the purpose of this invention is to provide the water-based of a kind of good antirust property and environmental protection.
The present invention mainly uses organic constituent to design the metal antirusting agent of water-based.
In one aspect, the present invention provides a kind of water-based antirust agent, and it contains the water of 5～30wt% hexahydroaniline Citrate trianion, 0.2～5.0wt% benzotriazole, 2～12wt% polyoxyethylene glycol and surplus.
Preferably, water-based antirust agent contains the water of 10～15wt% hexahydroaniline Citrate trianion, 0.5～2.0wt% benzotriazole, 4～10wt% polyoxyethylene glycol and surplus.
The molecular weight of polyoxyethylene glycol is 200～20000 generally speaking, and is preferred 300～5000, more preferably 350～1000.
Particularly preferably, it also contains the substituted benzimidazole with following formula of 1-4wt% (preferred 1.5-3wt%):
For the present invention, under preferred situation, employed hexahydroaniline Citrate trianion is that purity is more than 97%, more than 98%, and the more preferably high purity hexahydroaniline Citrate trianion more than 99%.
Said in the present invention hexahydroaniline Citrate trianion preferably adopts the hexahydroaniline Citrate trianion through the method preparation that may further comprise the steps:
(1) gets Hydrocerol A, add the complete after-filtration clarification of pure water heating for dissolving;
(2) in the hexahydroaniline of respective amount, the citric acid solution after adding slowly adding while stirring and filtering makes both 60～90 ℃ of fully reactions down, and adding hexahydroaniline or Hydrocerol A at last, to transfer pH be 7.5～9;
(3) heating concentrates, and ends until epitaxial occurring, while hot hot soln is cooled off;
(4) refrigerative hexahydroaniline Citrate trianion is dried.
Preferably, the mol ratio of hexahydroaniline in the step (2) and Hydrocerol A is 3.1: 1～3.3: 1.
Preferably, the temperature of reaction in the step (2) is that the stirring velocity in 75～80 ℃ and the step (2) is 50～100r/min.
Preferably, the cooling in the step (3) comprises while hot hot soln being poured on and is cooled to bulk in the plate.
Preferably, the oven dry in the step (4) comprise with blocky hexahydroaniline Citrate trianion in the plate do into fritter under 80～95 ℃, dry product.
The reaction of above step (2) is following:
C
6H
8O
7+3NH
2C
6H
11→(C
6H
13N)
3·C
6H
8O
7。
Further preferably, the described bake out temperature of step (4) is 85 ℃.
The preparation method of hexahydroaniline Citrate trianion of the present invention has following advantage and effect:
(1) the prepared hexahydroaniline Citrate trianion purity that obtains of the inventive method is high, foreign ion is few.
(2) simple, the less energy consumption, with low cost of the inventive method technology.
(3) it is block directly to put cold one-tenth after the prepared hexahydroaniline citrate solution that obtains of the inventive method concentrates, no mother liquor production, and yield is high, and environmental pollution is little.
Rust-preventive agent of the present invention can adopt methods such as direct immersion, spray that equipment and parts are carried out antirust processing.
The rust-preventive agent that contains hexahydroaniline Citrate trianion, benzotriazole, polyoxyethylene glycol and water of the present invention can be adsorbed on the metallic surface, forms continuous and firm adsorption layer, stops corrosive medium and metallic contact, thereby plays rust prevention.
Water-based antirust agent of the present invention has good rust-proof effect for metals such as iron, steel, iron alloy, aluminium, copper, can be used for the antirust of hardwares such as iron, steel, iron alloy, aluminium, copper and parts.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Preparation example 1
Take by weighing 210 gram monohydrate potassiums in the beaker of 1000mL, add 400mL pure water stirring and dissolving, the filtration clarification is subsequent use.In another 1000mL beaker, add 317 gram hexahydroaniline, under stirring (50r/min), slowly add and filter clarifying citric acid solution, under 80 ℃, react completely; This moment, solution was transparence, and pH value of solution is 8.5, and heating has been concentrated into epitaxial and has occurred; Dense crystalline substance is put cold one-tenth in clean plate block; Do into again fritter in 85 ℃ dry 4 hours down, product 451.4 grams, yield is 98.4%.Detect, content is 99.3% (with (C
6H
13N)
3C
6H
8O
7Meter), the content of C1, F, Br all＜10ppm.
Preparation example 2
Take by weighing 210 gram monohydrate potassiums in the beaker of 1000mL, add 400mL pure water stirring and dissolving, the filtration clarification is subsequent use.In another 1000mL beaker, add 307 gram hexahydroaniline, under stirring (50r/min), slowly add and filter clarifying citric acid solution, under 80 ℃, react completely; This moment, solution was transparence, and pH value of solution is 7.5, and heating has been concentrated into epitaxial and has occurred; Dense crystalline substance is put cold one-tenth in clean plate block; Do into again fritter in 80 ℃ dry 4 hours down, product 445.8 grams, yield is 97.2%.Detect, content is 99.1% (with (C
6H
13N)
3C
6H
8O
7Meter), the content of Cl, F, Br all＜10ppm.
Preparation example 3
Take by weighing 210 gram monohydrate potassiums in the beaker of 1000mL, add 400mL pure water stirring and dissolving, the filtration clarification is subsequent use.In another 1000mL beaker, add 327 gram hexahydroaniline, under stirring (50r/min), slowly add and filter clarifying citric acid solution, under 90 ℃, react completely; This moment, solution was transparence, and pH value of solution is 9, and heating has been concentrated into epitaxial and has occurred; Dense crystalline substance is put cold one-tenth in clean plate block; Do into again fritter in 95 ℃ dry 3 hours down, product 453.6 grams, yield is 98.9%.Detect, content is 99.3% (with (C
6H
13N)
3C
6H
8O
7Meter), the content of Cl, F, Br all＜10ppm.
Preparation example 4
Take by weighing 210 gram monohydrate potassiums in the beaker of 1000mL, add 400mL pure water stirring and dissolving, the filtration clarification is subsequent use.In another 1000mL beaker, add 322 gram hexahydroaniline, under stirring (100r/min), slowly add and filter clarifying citric acid solution, under 60 ℃, react completely; This moment, solution was transparence, and pH value of solution is 8.7, and heating has been concentrated into epitaxial and has occurred; Dense crystalline substance is put cold one-tenth in clean plate block; Do into again fritter in 85 ℃ dry 4 hours down, product 450.4 grams, yield is 98.2%.Detect, content is 99.2% (with (C
6H
13N)
3C
6H
8O
7Meter), the content of C1, F, Br all＜10ppm.
More than among each embodiment the measuring method of hexahydroaniline citrate content following:
Accurately take by weighing 0.5 gram sample, claim accurate to 0.0001 gram.Pressing among the GB/T608-1988 6.1 regulation measures.Wherein the E value in the calculation formula is 0.1632.
Embodiment 1
Measure hexahydroaniline Citrate trianion, 4g benzotriazole, 12g polyoxyethylene glycol (molecular weight 400) and the 100ml water of 20g preparation example 1 respectively, even at 45 ℃ of following thorough mixing of temperature, the water-based antirust agent of acquisition embodiment 1.The test piece of one-level grey cast iron was soaked 15 minutes in the water-based antirust agent of embodiment 2; Take out after drying; Dried test film is placed in 35 ℃, the constant temperature and constant humidity case of 90% humidity, 5 week the back take out samples and observe demonstration test piece 5 all no changes with SEM (sem).
Embodiment 2
Measure hexahydroaniline Citrate trianion, 4g benzotriazole, 12g polyoxyethylene glycol (molecular weight 800) and the 100ml water of 15g preparation example 2 respectively, even at 45 ℃ of following thorough mixing of temperature, the water-based antirust agent of acquisition embodiment 2.The test piece of one-level grey cast iron was soaked 15 minutes in the water-based antirust agent of embodiment 3, take out after drying, dried test film is placed in 35 ℃, the environment of 90% humidity, observes test piece 5 all no changes through SEM.
Embodiment 3
Measure hexahydroaniline Citrate trianion, 4g benzotriazole, 2g 2-methyl-6-hydroxyl-benzoglyoxaline, 12g polyoxyethylene glycol (molecular weight 400) and the 100ml water of 20g preparation example 1 respectively, even at 45 ℃ of following thorough mixing of temperature, the water-based antirust agent of acquisition embodiment 3.The test piece of one-level grey cast iron was soaked 15 minutes in the water-based antirust agent of embodiment 2, take out after drying, dried test film is placed in 35 ℃, the constant temperature and constant humidity case of 90% humidity, test piece 10 all no changes.
Embodiment 4
Measure hexahydroaniline Citrate trianion, 4g benzotriazole, 2g 2-methyl-6-amino-benzoglyoxaline, 12g polyoxyethylene glycol (molecular weight 400) and the 100ml water of 20g preparation example 3 respectively, even at 45 ℃ of following thorough mixing of temperature, the water-based antirust agent of acquisition embodiment 4.The test piece of one-level grey cast iron was soaked 15 minutes in the water-based antirust agent of embodiment 4, take out after drying, dried test film is placed in 35 ℃, the constant temperature and constant humidity case of 90% humidity, test piece 10 all no changes.
Can find out that from above result the water-based antirust agent that contains hexahydroaniline Citrate trianion of the present invention has good rust-proof effect.In addition, contain the benzoglyoxaline Citrate trianion and further improve antiseptic property.
Above-mentioned preparation example and embodiment are preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. water-based antirust agent, it contains the water of 5 ~ 30wt% hexahydroaniline Citrate trianion, 0.2 ~ 5.0wt% benzotriazole, 2 ~ 12wt% polyoxyethylene glycol and surplus.
2. water-based antirust agent according to claim 1, it contains the water of 10 ~ 15wt% hexahydroaniline Citrate trianion, 0.5 ~ 2.0wt% benzotriazole, 4 ~ 10wt% polyoxyethylene glycol and surplus.
3. water-based antirust agent according to claim 1 and 2, wherein the molecular weight of polyoxyethylene glycol is 200 ~ 20000.
4. according to each described water-based antirust agent of claim 1 ~ 3, it also contains the substituted benzimidazole of 1-4wt%:
5. water-based antirust agent according to claim 1 and 2, the purity of wherein said hexahydroaniline Citrate trianion are more than 97%.
6. water-based antirust agent according to claim 5, the method preparation of wherein said hexahydroaniline Citrate trianion through may further comprise the steps:
(1) gets Hydrocerol A, add the complete after-filtration clarification of pure water heating for dissolving;
(2) in the hexahydroaniline of respective amount, the citric acid solution after slowly adding is while stirring filtered makes both 60～90 ℃ of fully reactions down, and adding hexahydroaniline or Hydrocerol A at last, to transfer pH be 7.5～9;
(3) heating concentrates, and ends until epitaxial occurring, while hot hot soln is cooled off;
(4) refrigerative hexahydroaniline Citrate trianion is dried.
7. water-based antirust agent according to claim 6 is characterized in that, the hexahydroaniline in the step (2) and the mol ratio of Hydrocerol A are 3.1:1～3.3:1.
8. water-based antirust agent according to claim 6 is characterized in that, the temperature of reaction in the step (2) is that the stirring velocity in 75～80 ℃ and the step (2) is 50～100r/min.
9. water-based antirust agent according to claim 6 is characterized in that, the cooling in the step (3) comprises while hot hot soln being poured on and is cooled to bulk in the plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110230921A CN102296297B (en) | 2011-08-12 | 2011-08-12 | Aqueous metal anti-rust agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110230921A CN102296297B (en) | 2011-08-12 | 2011-08-12 | Aqueous metal anti-rust agent |
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|---|---|
| CN102296297A CN102296297A (en) | 2011-12-28 |
| CN102296297B true CN102296297B (en) | 2012-07-18 |
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| CN104562033A (en) * | 2014-09-30 | 2015-04-29 | 金寨县宏拓机电有限责任公司 | Antirust agent and preparation method thereof |
| CN107216938A (en) * | 2017-07-07 | 2017-09-29 | 荆门市拓达科技有限公司 | A kind of micro emulsion transformant metal rust-inhibiting liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1021063C (en) * | 1988-12-30 | 1993-06-02 | 杨延松 | Passivating liquid for steel and iron surface treatment |
| CN1786281A (en) * | 2005-12-14 | 2006-06-14 | 王开平 | Metal surface treatment agent |
| CN101130711A (en) * | 2006-08-23 | 2008-02-27 | 冯为民 | Method of producing water-based cutting fluid |
| CN100543190C (en) * | 2008-06-19 | 2009-09-23 | 广州嘉史洁环保科技有限公司 | A kind of metal antirusting agent |
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Granted publication date: 20120718 Termination date: 20130812 |