CN107419274A - A kind of antirust agent and preparation method thereof - Google Patents

A kind of antirust agent and preparation method thereof Download PDF

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Publication number
CN107419274A
CN107419274A CN201710721308.9A CN201710721308A CN107419274A CN 107419274 A CN107419274 A CN 107419274A CN 201710721308 A CN201710721308 A CN 201710721308A CN 107419274 A CN107419274 A CN 107419274A
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acid
antirust agent
preset temperature
temperature
preset
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CN107419274B (en
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胡文云
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Wuhan Polytechnic University
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Wuhan Polytechnic University
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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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/12—Reaction products
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06—Organic compounds derived from inorganic acids or metal salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/081—Biodegradable compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/66—Hydrolytic stability

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Lubricants (AREA)

Abstract

The present invention discloses a kind of antirust agent and preparation method thereof, and the antirust agent includes aliphatic acid, alcamine compound, boric acid and catalyst, and the mol ratio of the aliphatic acid, alcamine compound and boric acid is 5:2:1~1:1:1；The preparation method of the antirust agent includes：Aliphatic acid is put into reactor, heating stirring；When temperature rises to the first preset temperature, alcamine compound and catalyst are added, and open condensation reflux unit；When temperature rises to the second preset temperature, boric acid is added, continues to heat up；When temperature rises to three preset temperatures, the condensation reflux unit is closed, when being continuously heating to four preset temperatures, stops heating and being incubated；Insulation cools after terminating.Antirust agent prepared by the present invention, its antirust term of validity length, and there is good antiwear and antifriction ability, hydrolysis stability and biological degradability.

Description

A kind of antirust agent and preparation method thereof
Technical field
The present invention relates to field of metal surface treatment technology, more particularly to a kind of antirust agent and preparation method thereof.
Background technology
Because metalwork is easy to get rusty during production and processing and transport, it will usually make metal watch using antirust agent Face forms thin film, and corrosion of metal is caused to avoid metal from being contacted with moisture or other chemical compositions.External addition at present The antirust agent product of agent company production can reach preferable rust-proof effect, but because being monopolized by offshore company, it is expensive, and The antirust agent product of Domestic Additives manufacturer production is concentrated mainly on petroleum sulfonate, synthesising sulfonate, alkenyl succinic acid, alkenyl The antirust agent product such as succinate and natrium nitrosum, its long-term rust prevention effect against corrosion are not satisfactory.
The content of the invention
The main object of the present invention is to propose a kind of antirust agent and preparation method thereof, it is intended to improves the rust-preventing characteristic of antirust agent Energy.
To achieve the above object, a kind of antirust agent proposed by the present invention, including aliphatic acid, alcamine compound, boric acid with And catalyst for esterification reaction, wherein, the mol ratio of the aliphatic acid, alcamine compound and boric acid is 5:2:1~1:1:1.
Preferably, the addition of the catalyst for esterification reaction is that the aliphatic acid, alcamine compound and boric acid are total The 0.2~1% of quality.
Preferably, the aliphatic acid includes at least one of octanoic acid, capric acid, laurate and alkenyl succinic acid.
Preferably, the alcamine compound includes at least one of triethanolamine and diethanol amine.
Preferably, the catalyst for esterification reaction is included in tetra-n-butyl titanate, the concentrated sulfuric acid, hydrochloric acid and phosphoric acid at least It is a kind of.
The present invention also proposes a kind of preparation method of antirust agent described above, it is characterised in that comprises the following steps：
Aliphatic acid is put into reactor, heating stirring；
When temperature rises to the first preset temperature, alcamine compound and catalyst for esterification reaction are added, and open condensation Reflux；
When temperature rises to the second preset temperature, boric acid is added, continues to heat up；
When temperature rises to three preset temperatures, the condensation reflux unit is closed, is continuously heating to the 4th preset temperature When, stop heating and being incubated；
Insulation cools after terminating；
Wherein, the 4th preset temperature is higher than the 3rd preset temperature, and the 3rd preset temperature is higher than described the Two preset temperatures, second preset temperature are higher than first preset temperature.
Preferably, first preset temperature is 70~80 DEG C, and second preset temperature is 100~110 DEG C, described the Three preset temperatures are 132~136 DEG C, and the 4th preset temperature is 138~140 DEG C.
In technical solution of the present invention, antirust is prepared as raw material using aliphatic acid, alcamine compound and boric acid as antirust agent Agent, its antirust term of validity length, and there is certain antiwear and antifriction ability, antirust excellent combination property against corrosion, while also have Good cleaning, hydrolysis stability and biological degradability.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with Structure according to these accompanying drawings obtains other accompanying drawings.
Fig. 1 is the schematic flow sheet of an embodiment of the preparation method of antirust agent provided by the invention.
The realization, functional characteristics and advantage of the object of the invention will be described further referring to the drawings in conjunction with the embodiments.
Embodiment
It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
A kind of antirust agent proposed by the present invention, including aliphatic acid, alcamine compound, boric acid and esterification catalytic Agent, wherein, the mol ratio of the aliphatic acid, alcamine compound and boric acid is 5:2:1~1:1:1.
Antirust agent is prepared as raw material using aliphatic acid, alcamine compound and boric acid as antirust agent, passes through polarity therein Group absorption forms one layer of oil film in metal surface, so that by metal and air exclusion, prevents metal from corrosion occurs, described anti- The antirust term of validity length of rusty gold, and there is certain antiwear and antifriction ability, antirust excellent combination property against corrosion, while also have Good cleaning, hydrolysis stability and biological degradability.
Preferably, the addition of the catalyst for esterification reaction is that the aliphatic acid, alcamine compound and boric acid are total The 0.2~1% of quality.As a rule, addition of the catalyst in chemical reaction is usually no more than the 10% of raw material gross mass, In embodiments of the present invention, the addition of the catalyst for esterification reaction is the aliphatic acid, alcamine compound and boric acid The 0.2~1% of gross mass, you can promote the quick progress of esterification, improve reaction efficiency.
Preferably, the aliphatic acid includes at least one of octanoic acid, capric acid, laurate and alkenyl succinic acid.Some The compound of fatty acid after over-churning can obtain that the antirust agent of oil film can be generated in metal surface, its aliphatic acid Species is different, and the rust-proof effect of the ester of generation would also vary from, wherein, octanoic acid, capric acid, laurate and alkenyl succinic acid life Into ester rust-proof effect it is ideal.
Preferably, the alcamine compound includes at least one of triethanolamine and diethanol amine.Nitrogen-atoms is that have Most common hetero atom in machine corrosion inhibiter, it will be used to prepare antirust agent with the alcamine compound containing N structure, can strengthen The antirust resistance to corrosion of antirust agent.
Preferably, the catalyst for esterification reaction is included in tetra-n-butyl titanate, the concentrated sulfuric acid, hydrochloric acid and phosphoric acid at least It is a kind of.Under normal circumstances, antirust agent is easy to cause antirust to fail due to rupture in the oil film that metalwork surface is formed, this hair In bright technical scheme, the addition of boric acid can improve the post bake toughness of Rust Preventing Oil Film, and the oil film for forming metal surface is not fragile Split, so as to increase the rust-proof effect of the antirust agent.
Wherein, the concentrated sulfuric acid, hydrochloric acid and phosphoric acid are the conventional catalyst of esterification, can promote esterification Carry out, the tetra-n-butyl titanate is moderate performance as the characteristics of catalyst for esterification reaction, and addition is few, can avoid because The addition of vigorous reaction or catalyst is excessive and influences the performance of esterification reaction product, therefore with choosing in technical solution of the present invention By the use of tetra-n-butyl titanate as based on catalyst.
Further, since benzene ring structure is not contained in all raw materials selected in technical solution of the present invention, so prepare The antirust agent also has certain biological degradability, can be degraded by microorganisms after the antirust agent goes out of use, and is a kind of Green product.
The present invention also proposes a kind of preparation method of antirust agent described above, wherein, the preparation method bag of the antirust agent Include following steps：
Step S10, aliphatic acid is put into reactor, heating stirring；
Wherein described reactor can be selected tank reactor etc. and be provided with heating and agitating device in industrial processes Reaction unit；When being tested in the lab, the experimental apparatus such as three-necked flask, condenser pipe, stirring rod can be selected and build simply Reaction unit, to realize the purpose that is heated up and stirred to reaction raw materials.
Step S20, when temperature rises to the first preset temperature, alcamine compound and catalyst for esterification reaction are added, and Open condensation reflux unit；
Step S30, when temperature rises to the second preset temperature, boric acid is added, continues to heat up；
Step S40, when temperature rises to three preset temperatures, the condensation reflux unit is closed, is continuously heating to the 4th During preset temperature, stop heating and being incubated；
Step S50, insulation cools after terminating.
Alternatively, first preset temperature is 70~80 DEG C, and second preset temperature is 100~110 DEG C, described the Three preset temperatures are 132~136 DEG C, and the 4th preset temperature is 138~140 DEG C.When the raw material selected by esterification not Meanwhile the temperature setting in each stage may also be different in course of reaction, actual temp sets the classification of visual response thing and to generation Depending on the demand of thing.
Alternatively, described cool can naturally cool to room temperature, can also be by opening condensation reflux unit, together When stirred, by reaction product accelerate be cooled to room temperature.
The antirust agent prepared by the above method, metalwork can be carried out at antirust or derusting separately as antirust agent Reason, can also be added in lubricating oil and use, make lubricating oil be provided simultaneously with lubrication, cleaning rust-proof the effect of.
In order that the preparation technology and its rustless property of antirust agent provided by the invention are more directly perceived, it is real with reference to application Example is applied to illustrate with comparative example：
Specific embodiment 1
(1) octanoic acid, triethanolamine, boric acid and tetra-n-butyl titanate are weighed, wherein, octanoic acid, triethanolamine and boric acid Mol ratio is 5:2:1, the quality of tetra-n-butyl titanate is the 1.0% of octanoic acid, triethanolamine and boric acid gross mass；Then by octanoic acid Put into three-necked flask, open heater and agitating device carries out heating stirring；
(2) when temperature rises to 75 DEG C, the triethanolamine and tetra-n-butyl titanate weighed is added, and open and connect with condenser pipe Logical water pipe, carry out condensing reflux；
(3) when temperature rises to 105 DEG C, the boric acid weighed is added, continues to heat up；
(4) when temperature rises to 135 DEG C, the water pipe connected with condenser pipe is closed, while be continuously heating to stop at 139 DEG C Heating, it is incubated 30min；
(5) after insulation terminates, agitating device is opened, and opens the water pipe connected with condenser pipe and carries out condensing reflux, so that Product accelerates to be cooled to room temperature, finally discharging packaging.
Specific embodiment 2
(2) octanoic acid, triethanolamine, boric acid and tetra-n-butyl titanate are weighed, wherein, octanoic acid, triethanolamine and boric acid Mol ratio is 2:1:1, the quality of tetra-n-butyl titanate is the 0.5% of octanoic acid, triethanolamine and boric acid gross mass；Then by octanoic acid Put into three-necked flask, open heater and agitating device carries out heating stirring；
(2) when temperature rises to 75 DEG C, the triethanolamine and tetra-n-butyl titanate weighed is added, and open and connect with condenser pipe Logical water pipe, carry out condensing reflux；
(3) when temperature rises to 105 DEG C, the boric acid weighed is added, continues to heat up；
(4) when temperature rises to 135 DEG C, the water pipe connected with condenser pipe is closed, while be continuously heating to stop at 139 DEG C Heating, it is incubated 30min；
(5) after insulation terminates, agitating device is opened, and opens the water pipe connected with condenser pipe and carries out condensing reflux, so that Product accelerates to be cooled to room temperature, finally discharging packaging.
Specific embodiment 3
(3) octanoic acid, triethanolamine, boric acid and tetra-n-butyl titanate are weighed, wherein, octanoic acid, triethanolamine and boric acid Mol ratio is 1:1:1, the quality of tetra-n-butyl titanate is the 0.2% of octanoic acid, triethanolamine and boric acid gross mass；Then by octanoic acid Put into three-necked flask, open heater and agitating device carries out heating stirring；
(2) when temperature rises to 75 DEG C, the triethanolamine and tetra-n-butyl titanate weighed is added, and open and connect with condenser pipe Logical water pipe, carry out condensing reflux；
(3) when temperature rises to 105 DEG C, the boric acid weighed is added, continues to heat up；
(4) when temperature rises to 135 DEG C, the water pipe connected with condenser pipe is closed, while be continuously heating to stop at 139 DEG C Heating, it is incubated 30min；
(5) after insulation terminates, agitating device is opened, and opens the water pipe connected with condenser pipe and carries out condensing reflux, so that Product accelerates to be cooled to room temperature, finally discharging packaging.
Using commercially available T746 antirust agent as comparative example, T746 antirust agent also known as T746 (dodecenylsuccinic acid).
Every physical and chemical index of 1 each embodiment of table and comparative example product
The antirust agent and commercially available T746 antirust agent prepared to the various embodiments described above carries out corresponding performance test, its items reason Change index and method of testing is as shown in table 1, from table 1 it follows that in copper corrosion performance test, the present embodiment product Corrosion resistance is better than T746 antirust agent, and can be dissolved each other with water with arbitrary proportion, illustrates antirust prepared by the embodiment of the present invention The antirust etch resistant properties of agent are preferable, and due to can be miscible with water, caused liquid waste processing in the production process of the antirust agent Get up more convenient.Meanwhile after antirust treatment is carried out to metalwork, the antirust agent remained on metalwork can be used directly Water rinses out, so as to have good cleaning.
The antiwear and antifriction ability and hydrolysis stability test result of the embodiment product of table 2
For handling the oil product (such as lubricating oil, base oil, antirust agent etc.) of metalwork, the antiwear and antifriction energy of product Power and hydrolysis stability are also the important parameter for weighing properties of product.Therefore, also antirust agent provided by the invention is resisted The performance test of the ability of rubbing and hydrolysis stability is worn away, specific method of testing is：The antirust agent prepared by above-described embodiment is pressed The addition of 2% (mass fraction) is added in base oil, tests its antiwear and antifriction ability and hydrolysis stability respectively, and it tests knot Fruit and method of testing are as shown in table 2.For T746 antirust agent, itself is simultaneously stable without antiwear and antifriction ability and hydrolysis Property, and antirust agent provided by the invention is due to wherein with the addition of boracic and containing nitrogen compound, having good antiwear and antifriction energy Power and hydrolysis stability, so as to have more preferable antirust resistance to corrosion.
The preferred embodiments of the present invention are these are only, are not intended to limit the scope of the invention, it is every to utilize this hair The equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related skills Art field, is included within the scope of the present invention.

Claims (7)

  1. A kind of 1. antirust agent, it is characterised in that including aliphatic acid, alcamine compound, boric acid and catalyst for esterification reaction, its In, the mol ratio of the aliphatic acid, alcamine compound and boric acid is 5:2:1~1:1:1.
  2. 2. antirust agent as claimed in claim 1, it is characterised in that the addition of the catalyst for esterification reaction is the fat The 0.2~1% of sour, alcamine compound and boric acid gross mass.
  3. 3. antirust agent as claimed in claim 1, it is characterised in that the aliphatic acid includes octanoic acid, capric acid, laurate and alkene At least one of base succinic acid.
  4. 4. antirust agent as claimed in claim 1, it is characterised in that the alcamine compound includes triethanolamine and diethanol At least one of amine.
  5. 5. antirust agent as claimed in claim 1, it is characterised in that the catalyst for esterification reaction include tetra-n-butyl titanate, At least one of the concentrated sulfuric acid, hydrochloric acid and phosphoric acid.
  6. 6. the preparation method of a kind of antirust agent as described in claim 1 to 5 any one, it is characterised in that including following step Suddenly：
    Aliphatic acid is put into reactor, heating stirring；
    When temperature rises to the first preset temperature, alcamine compound and catalyst for esterification reaction are added, and open condensing reflux Device；
    When temperature rises to the second preset temperature, boric acid is added, continues to heat up；
    When temperature rises to three preset temperatures, the condensation reflux unit is closed, when being continuously heating to four preset temperatures, is stopped Only heat and be incubated；
    Insulation cools after terminating；
    Wherein, the 4th preset temperature is higher than the 3rd preset temperature, and the 3rd preset temperature is pre- higher than described second If temperature, second preset temperature is higher than first preset temperature.
  7. 7. the preparation method of antirust agent as claimed in claim 6, it is characterised in that first preset temperature is 70~80 DEG C, second preset temperature is 100~110 DEG C, and the 3rd preset temperature is 132~136 DEG C, the 4th preset temperature For 138~140 DEG C.
CN201710721308.9A 2017-08-21 2017-08-21 A kind of antirust agent and preparation method thereof Active CN107419274B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108192691A (en) * 2018-02-06 2018-06-22 周文辽 A kind of preparation method of lubricating and antirust compositions of additives
CN108192691B (en) * 2018-02-06 2021-05-14 邯郸市宁龙润滑油添加剂有限公司 Preparation method of lubricating and antirust additive composition

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