CN105198749A - Citric acid polyol ester for rust prevention of black metal, water-based antirust agent and preparation method thereof - Google Patents
Citric acid polyol ester for rust prevention of black metal, water-based antirust agent and preparation method thereof Download PDFInfo
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- CN105198749A CN105198749A CN201510564084.6A CN201510564084A CN105198749A CN 105198749 A CN105198749 A CN 105198749A CN 201510564084 A CN201510564084 A CN 201510564084A CN 105198749 A CN105198749 A CN 105198749A
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- citric acid
- polyol ester
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- acid polyol
- ferrous metal
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/67—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids
- C07C69/675—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids of saturated hydroxy-carboxylic acids
- C07C69/704—Citric acid esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/62—Treatment of iron or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention relates to a citric acid polyol ester for rust prevention of black metal, a water-based antirust agent and a preparation method thereof. The citric acid polyol ester for rust prevention of the black metal is prepared by adopting citric acid and sorbitol as raw materials, anhydrous sodium acetate as a catalyst, and xylene as a solvent through esterification reaction; the water-based antirust agent is prepared by the citric acid polyol ester, sodium polyacrylate, diethylene glycol, cocamidopropyl betaine, polyethylene glycol monooleate, ammonium molybdate, sodium carbonate and pure water. The preparation method of the citric acid polyol ester for rust prevention is simple, environmental-friendly and low in cost; the black metal water-based antirust agent prepared by adopting the citric acid polyol ester as the main raw materials has the excellent effects of low cost, long rust prevention time (up to 8 months), no color and no toxin.
Description
Technical field
The present invention relates to ferrous metal surface protection field, be specifically related to the preparation method of the antirust citric acid polyol ester of a kind of ferrous metal and water-based antirust thereof.
Background technology
Current ferrous metal is the most general metal material of industrial application, and they are in storage process, can react with the oxygen in air, water etc. and produce corrosion.Early stage people mainly seal up for safekeeping these ferrous metal component by slushing oil, to reaching the object that metal surface and oxygen, water etc. are isolated, preventing or delaying metal generation corrosion.But because slushing oil is not easily removed in these ferrous metal component post-production processes, have impact on its subsequent processing operations, bring inconvenience to production.In order to overcome slushing oil drawback in this respect, in recent years, water-based antirust is owing to having antirust function good a middle or short term, and film-forming water soluble is better, washing is easy to removing, and do not affect ferrous metal component following process, thus water-based antirust production development is rapid.
Early stage water-based antirust is many containing highly toxic substance nitrite, and usually separates out white powder at ferrous metal surface after drying, and rustless property declines.ZL20131065780.0 adopts diglycolamine, tartrate etc. to form composite membrane-forming material, not containing nitrite, solve the problem that water-based antirust is antirust to ferrous metal preferably, but, due to the main film forming substance that diglycolamine is this water-based antirust, after the drying and forming-film of metallic surface, diglycolamine easily causes antirust rete xanthochromia, have impact on metallic surface appearance on the one hand, also can affect the water-soluble of antirust rete on the other hand, before making ferrous metal post-production, the removal difficulty of anti-rust film becomes large.
Summary of the invention
In order to overcome the above-mentioned problems in the prior art, the invention provides a kind of ferrous metal antirust citric acid polyol ester water-based antirust and preparation method thereof.This water-based antirust with citric acid polyol ester for main film forming substance, applicable various ferrous metal component medium-term and long-term antirust.
For achieving the above object, the technical solution used in the present invention is as follows:
The antirust citric acid polyol ester of a kind of ferrous metal, it is characterized in that: the antirust citric acid polyol ester of described ferrous metal is synthesized by following steps method: with citric acid and Sorbitol Powder for reaction raw materials, anhydrous sodium acetate is catalyzer, dimethylbenzene is reaction solvent, be prepared under temperature is 120-150 DEG C of condition, wherein, the mol ratio of citric acid and Sorbitol Powder is 0.3:1-0.8:1, the addition of anhydrous sodium acetate is 2% of citric acid quality, reaction times is 4-6h, question response thing acid number is less than 5mgKOH/g, stopped reaction, remove xylene solvent, cooling discharge obtains the antirust citric acid polyol ester of described ferrous metal.
Preferably, esterification reaction temperature is 130-140 DEG C, and the mol ratio of citric acid and Sorbitol Powder is 0.4:1-0.6:1, and the reaction times is 5h.
More preferably, esterification reaction temperature is 137 DEG C, and the mol ratio of citric acid and Sorbitol Powder is 0.5:1, and the reaction times is 5h.
A kind of ferrous metal water-based antirust, it is characterized in that: described water-based antirust is made up of following raw material and quality proportioning forms, wherein, citric acid polyol ester 20-35 part, sodium polyacrylate 4-8 part, Diethylene Glycol 5-15 part, AMONYL 380LC 0.5-1.5 part, polyethylene glycol monooleate 2-4 part, ammonium molybdate 1-2 part, sodium carbonate 0.5-1.5 part, pure water 33-67 part.
Preferably, the antirust citric acid polyol ester of ferrous metal that citric acid polyol ester adopts technique scheme of the present invention obtained, wherein, citric acid polyol ester 30 parts, sodium polyacrylate 5 parts, Diethylene Glycol 8 parts, AMONYL 380LC 1 part, polyethylene glycol monooleate 2 parts, ammonium molybdate 2 parts, 1 part, sodium carbonate, pure water 60 parts.
A kind of preparation method of ferrous metal water-based antirust, it is characterized in that: comprise the following steps: (1), add in reactor by the pure water of formula ratio, citric acid polyol ester, sodium polyacrylate, AMONYL 380LC, polyethylene glycol monooleate, stirring at normal temperature is until all dissolve; (2), by formula ratio add and add ammonium molybdate, sodium carbonate successively, be warming up to 40 DEG C, be stirred to after dissolving completely, then add the Diethylene Glycol of formula ratio, mix rear cooling discharge.
Beneficial effect of the present invention is: ferrous metal antirust citric acid polyol ester preparation method is simple, nontoxic, cost is low, because citric acid polyol ester of the present invention is main raw material and all the other additive compatibilities, synergy, the ferrous metal water-based antirust obtained is made to have the good result of antirust time long (antirust time was up to more than 8 months), product long storage time is all colourless, cost is low, not containing nitrite and phosphoric, nontoxic pollution-free.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: the preparation of the antirust citric acid polyol ester of ferrous metal, (1) citric acid of 30mol, the Sorbitol Powder of 100mol are added in reactor, add the anhydrous acetic acid sodium catalyst of citric acid quality 2% again, appropriate xylene solvent, mix and blend; (2) be warming up to 120 DEG C and carry out reaction 6h, product acid number is 4.6mgKOH/g, and namely removed under reduced pressure dimethylbenzene obtain citric acid polyol ester A.
Embodiment 2: the preparation of the antirust citric acid polyol ester of ferrous metal, (1) citric acid of 80mol, the Sorbitol Powder of 100mol are added in reactor, add the anhydrous acetic acid sodium catalyst of citric acid quality 2% again, appropriate xylene solvent, mix and blend; (2) about being warming up to xylene boiling point, (150 DEG C) carry out back flow reaction 4h, and product acid number is 3.4mgKOH/g, and namely removed under reduced pressure dimethylbenzene obtain citric acid polyol ester B.
Embodiment 3: the preparation of the antirust citric acid polyol ester of ferrous metal, (1) citric acid of 50mol, the Sorbitol Powder of 100mol are added in reactor, add the anhydrous acetic acid sodium catalyst of citric acid quality 2% again, appropriate xylene solvent, mix and blend; (2) about being warming up to xylene boiling point, (135 DEG C) carry out back flow reaction 5h, and product acid number is 3.8mgKOH/g, and namely removed under reduced pressure dimethylbenzene obtain citric acid polyol ester C.
Embodiment 4: citric acid polyol ester A, B, C of adopting embodiment 1-3 obtained are respectively for the preparation of ferrous metal water-based antirust.
(1), with the obtained citric acid polyol ester A of embodiment 1 for raw material time: ferrous metal water-based antirust a1 is made up of following raw material and quality proportioning forms, citric acid polyol ester 20Kg, sodium polyacrylate 4Kg, Diethylene Glycol 5Kg, AMONYL 380LC 0.5Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 1Kg, sodium carbonate 0.5Kg, pure water 33Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 1 below:
Table 1
Ferrous metal water-based antirust a2 is made up of following raw material and quality proportioning forms, citric acid polyol ester 35Kg, sodium polyacrylate 8Kg, Diethylene Glycol 15Kg, AMONYL 380LC 1.5Kg, polyethylene glycol monooleate 4Kg, ammonium molybdate 2Kg, sodium carbonate 1.5Kg, pure water 67Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 2 below:
Table 2
Ferrous metal water-based antirust a3 is made up of following raw material and quality proportioning forms, citric acid polyol ester 30Kg, sodium polyacrylate 5Kg, Diethylene Glycol 8Kg, AMONYL 380LC 1Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 2Kg, sodium carbonate 1Kg, pure water 60Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 3 below:
Table 3
(2), with the obtained citric acid polyol ester B of embodiment 2 for raw material time: ferrous metal water-based antirust b1 is made up of following raw material and quality proportioning forms, citric acid polyol ester 20Kg, sodium polyacrylate 4Kg, Diethylene Glycol 5Kg, AMONYL 380LC 0.5Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 1Kg, sodium carbonate 0.5Kg, pure water 33Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 4 below:
Table 4
Ferrous metal water-based antirust b2 is made up of following raw material and quality proportioning forms, citric acid polyol ester 35Kg, sodium polyacrylate 8Kg, Diethylene Glycol 15Kg, AMONYL 380LC 1.5Kg, polyethylene glycol monooleate 4Kg, ammonium molybdate 2Kg, sodium carbonate 1.5Kg, pure water 67Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 5 below:
Table 5
Ferrous metal water-based antirust b3 is made up of following raw material and quality proportioning forms, citric acid polyol ester 30Kg, sodium polyacrylate 5Kg, Diethylene Glycol 8Kg, AMONYL 380LC 1Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 2Kg, sodium carbonate 1Kg, pure water 60Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 6 below:
Table 6
Three, with the obtained citric acid polyol ester C of embodiment 3 for raw material time: ferrous metal water-based antirust c1 is made up of following raw material and quality proportioning forms, citric acid polyol ester 20Kg, sodium polyacrylate 4Kg, Diethylene Glycol 5Kg, AMONYL 380LC 0.5Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 1Kg, sodium carbonate 0.5Kg, pure water 33Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 7 below:
Table 7
Ferrous metal water-based antirust c2 is made up of following raw material and quality proportioning forms, citric acid polyol ester 35Kg, sodium polyacrylate 8Kg, Diethylene Glycol 15Kg, AMONYL 380LC 1.5Kg, polyethylene glycol monooleate 4Kg, ammonium molybdate 2Kg, sodium carbonate 1.5Kg, pure water 67Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 8 below:
Table 8
Ferrous metal water-based antirust c3 is made up of following raw material and quality proportioning forms, citric acid polyol ester 30Kg, sodium polyacrylate 5Kg, Diethylene Glycol 8Kg, AMONYL 380LC 1Kg, polyethylene glycol monooleate 2Kg, ammonium molybdate 2Kg, sodium carbonate 1Kg, pure water 60Kg.Get above-mentioned water-based antirust to detect by required standard, technical indicator is as shown in table 9 below:
Table 9
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., be all included within protection scope of the present invention.
Claims (5)
1. the antirust citric acid polyol ester of ferrous metal, it is characterized in that: the antirust citric acid polyol ester of described ferrous metal is synthesized by following methods: with citric acid and Sorbitol Powder for reaction raw materials, anhydrous sodium acetate is catalyzer, dimethylbenzene is reaction solvent, be prepared under temperature is 120-150 DEG C of condition, wherein, the mol ratio of citric acid and Sorbitol Powder is 0.3:1-0.8:1, preferred molar ratio is 0.5:1, the addition of anhydrous sodium acetate is 2% of citric acid quality, reaction times is 4-6h, preferred 5h, question response thing acid number is less than 5mgKOH/g, stopped reaction, remove xylene solvent, cooling discharge obtains the antirust citric acid polyol ester of described ferrous metal.
2. a ferrous metal water-based antirust, it is characterized in that: described water-based antirust is made up of following raw material and quality proportioning forms, wherein, citric acid polyol ester 20-35 part, sodium polyacrylate 4-8 part, Diethylene Glycol 5-15 part, AMONYL 380LC 0.5-1.5 part, polyethylene glycol monooleate 2-4 part, ammonium molybdate 1-2 part, sodium carbonate 0.5-1.5 part, pure water 33-67 part.
3. ferrous metal water-based antirust as claimed in claim 2, is characterized in that: described citric acid polyol ester is the antirust citric acid polyol ester of ferrous metal according to claim 1.
4. ferrous metal water-based antirust as claimed in claim 3, is characterized in that: citric acid polyol ester 30 parts, sodium polyacrylate 5 parts, Diethylene Glycol 8 parts, AMONYL 380LC 1 part, polyethylene glycol monooleate 2 parts, ammonium molybdate 2 parts, 1 part, sodium carbonate, pure water 60 parts.
5. the preparation method of a ferrous metal water-based antirust as claimed in claim 2, it is characterized in that: comprise the following steps: (1), add in reactor by the pure water of formula ratio, citric acid polyol ester, sodium polyacrylate, AMONYL 380LC, polyethylene glycol monooleate, stirring at normal temperature is until all dissolve; (2), by formula ratio add and add ammonium molybdate, sodium carbonate successively, be warming up to 40 DEG C, be stirred to after dissolving completely, then add the Diethylene Glycol of formula ratio, mix rear cooling discharge.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418651A (en) * | 2017-08-30 | 2017-12-01 | 黄山学院 | A kind of heptyl ester calcium salt detergent for lubricating oil of carboxylated citric acid three and preparation method thereof |
| CN115261866A (en) * | 2022-08-02 | 2022-11-01 | 黄山学院 | Long-acting thick-film water-based antirust agent and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418651A (en) * | 2017-08-30 | 2017-12-01 | 黄山学院 | A kind of heptyl ester calcium salt detergent for lubricating oil of carboxylated citric acid three and preparation method thereof |
| CN107418651B (en) * | 2017-08-30 | 2020-02-14 | 黄山学院 | Carboxylated triheptyl citrate calcium salt lubricating oil detergent and preparation method thereof |
| CN115261866A (en) * | 2022-08-02 | 2022-11-01 | 黄山学院 | Long-acting thick-film water-based antirust agent and preparation method thereof |
| CN115261866B (en) * | 2022-08-02 | 2023-12-19 | 黄山学院 | Long-acting thick film water-based antirust agent and preparation method thereof |
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Effective date of registration: 20200721 Address after: 239238 Wuyi Park, Nanqiao Industrial Development Zone, Chuzhou City, Anhui Province Patentee after: Chuzhou lianjiang Environmental Protection Technology Co., Ltd Address before: 245041 No. 39 West Sea Road, Tunxi District, Anhui, Huangshan City Patentee before: HUANGSHAN University |