CN113322120A - Production and preparation method of annealing cleaning volatile auxiliary for aluminum alloy strip rolling oil - Google Patents

Production and preparation method of annealing cleaning volatile auxiliary for aluminum alloy strip rolling oil Download PDF

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CN113322120A
CN113322120A CN202110726183.5A CN202110726183A CN113322120A CN 113322120 A CN113322120 A CN 113322120A CN 202110726183 A CN202110726183 A CN 202110726183A CN 113322120 A CN113322120 A CN 113322120A
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parts
preparation
aluminum alloy
temperature
alloy strip
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CN113322120B (en
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周鑫
游江海
刘润杰
杨金兵
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Jiangsu Pinhe Petroleum Technology Co ltd
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Jiangsu Pinhe Petroleum Technology Co ltd
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Abstract

The invention discloses a production and preparation method of an annealing cleaning volatilization auxiliary agent for aluminum alloy strip rolling oil, which is prepared by the provided raw materials and a specific process, wherein the performance of the volatilization auxiliary agent is improved by introducing a reflux device and an electrochemical reaction device, the volatilization performance of the volatilization auxiliary agent is essentially improved from a compound, meanwhile, hydroxyl ions are ionized from phenol through electrochemistry, S elements in an aluminum alloy strip can be further removed by integrating other reactants in the annealing process, and the surface performance of a plate is improved.

Description

Production and preparation method of annealing cleaning volatile auxiliary for aluminum alloy strip rolling oil
Technical Field
The invention relates to the technical field of aluminum alloy oil-making additives, in particular to a production and preparation method of an annealing cleaning volatile additive for aluminum alloy strip rolling oil.
Background
The aluminum alloy plate strip is used as an important nonferrous metal processing material, and the dosage of the aluminum alloy plate strip in a metal strip is only lower than that of steel. In the process of rolling aluminum alloy, generally, a rough-rolled aluminum alloy plate produced by hot rolling is subjected to cold rolling processing for a plurality of times, and is pressed into an aluminum alloy sheet with smaller thickness until the thickness is less than 0.2 mm. Along with the sustainable development of Chinese economy and the upgrading of industrial transformation, the quality requirement of the market on aluminum alloy plate strip products is increasingly improved, and the process lubrication effect in the processing process of the aluminum alloy plate strip plays a key role in the production efficiency, equipment loss and plate product quality of enterprises and is more and more emphasized.
The rolling oil liquid of the aluminum alloy plate strip is mainly divided into hot rolling emulsion and cold rolling oil, wherein during hot rolling, oil-in-water (O/W) emulsion oil is generally adopted for cooling and lubricating, and the cold rolling oil is generally pure oil. Particularly, the good cold rolling oil needs to have the requirements of no toxicity, low odor, low viscosity, high flash point, low final boiling point, narrow fraction, good viscosity-temperature performance, no oil spot during annealing, good oxidation stability, good surface smoothness and the like. In the original rolling oil, the base oil usually accounts for about 94-95%, and with the enhancement of environmental awareness and cold rolling technology, the cold rolling of the aluminum alloy plate and strip develops towards the directions of large rolling reduction, low oil consumption, high speed and high surface quality, and has stricter requirements on the volatilization performance and the annealing cleaning performance of the aluminum alloy cold rolling oil.
The existing annealing cleaning volatilization auxiliary agent for the aluminum alloy strip rolling oil is insufficient in volatilization performance and annealing cleaning performance, and in consideration of the fact that the aluminum alloy strip is developed towards a high-performance medium plate and a more precise aluminum foil in the future, the product needs to have better surface quality of a finished product, and the aluminum alloy cold rolling oil needs to have more proper viscosity, lower aromatic hydrocarbon and sulfur content, narrower fraction, higher flash point and lower oil consumption, so that the research on the novel annealing cleaning volatilization auxiliary agent for the aluminum alloy strip rolling oil is of great significance.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention is provided in view of the problems of the annealing cleaning volatile assistant for the existing aluminum alloy strip rolling oil.
Therefore, the technical problem solved by the invention is as follows: solves the problem that the existing annealing cleaning volatilization auxiliary agent for the rolling oil of the aluminum alloy strip has insufficient volatilization performance and annealing cleaning performance.
In order to solve the technical problems, the invention provides the following technical scheme: a production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 10-15 parts of synthetic ester, 5-7 parts of emulsifier compound, 1-2 parts of dissolving agent, 10-15 parts of ethyl acetate, 5-7 parts of curing agent, 3-5 parts of organic binder, 5-10 parts of activated carbon powder, 10-13 parts of phenol, 15-20 parts of potassium permanganate solution with the concentration of 0.1mol/l, 5-8 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and a 60% polar solvent into an electrochemical reaction device, slowly dripping a potassium permanganate solution into the electrochemical reaction device at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of a reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring for 3 hours at a maintained temperature after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1:1.4 or 1:1.5 or 1: 1.8.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the emulsifier complex comprises polyethylene glycol type nonionic surfactant and anionic surfactant, wherein the weight ratio of the polyethylene glycol type nonionic surfactant to the anionic surfactant is 1: 2, compounding and mixing.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the nonionic surfactant is polyoxyethylene amide formed by addition of hydroxyl-containing castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the curing agent is any one of sorbate, sorbamide, sodium silicate and zinc fluoborate.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the organic adhesive comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the polar solvent is one or a mixture of more of DPG, PG and DPMA.
As a preferred scheme of the production and preparation method of the annealing cleaning volatile assistant for the rolling oil of the aluminum alloy strip, the method comprises the following steps: the preparation method comprises the following steps of adding 20-25 parts of hot-melt high-temperature granules and 1-2 parts of film forming agents into a reaction kettle, adding the hot-melt high-temperature granules, the film forming agents and 20% of organic binders into the reaction kettle, cooling to room temperature after hot melting at 200 ℃, adding the annealing and cleaning volatile auxiliary agents and 40% of polar solvents, and preparing the dispersion net bag with the dispersion mesh determined as the target mesh for use.
The invention has the beneficial effects that: the invention provides a production and preparation method of an annealing cleaning volatilization auxiliary agent for aluminum alloy strip rolling oil, which is prepared by the provided raw materials and a specific process, wherein the performance of the volatilization auxiliary agent is improved by introducing a reflux device and an electrochemical reaction device, the volatilization performance of the volatilization auxiliary agent is essentially improved from a compound, meanwhile, hydroxyl ions are ionized from phenol through electrochemistry, S elements in an aluminum alloy strip can be further removed by integrating other reactants in the annealing process, and the surface performance of a plate is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a flow chart of a preparation method provided by the present invention.
Fig. 2 is a schematic diagram of the production of a mesh pouch according to the present invention.
Fig. 3 is a partial method view of a mesh pouch provided by the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, shall fall within the protection scope of the present invention.
The existing annealing cleaning volatile assistant for the aluminum alloy strip rolling oil has insufficient volatility and annealing cleaning performance.
Therefore, the invention provides a production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil, which comprises the following steps.
Example (b):
example 1
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 10 parts of synthetic ester, 5 parts of emulsifier compound, 1 part of dissolving agent, 10 parts of ethyl acetate, 5 parts of curing agent, 3 parts of organic adhesive, 5 parts of activated carbon powder, 10 parts of phenol, 15 parts of potassium permanganate solution with the concentration of 0.1mol/l, 5 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
Wherein the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1: 1.4.
Wherein the emulsifier compound comprises polyethylene glycol type nonionic surfactant and anionic surfactant in a ratio of 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
Wherein, the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
Wherein the curing agent is sorbate.
Further, the organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
Wherein the polar solvent is one or a mixture of more of DPG, PG and DPMA.
Furthermore, the preparation method comprises 20 parts of hot-melt high-temperature granules and 1 part of film forming agent, wherein the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive are added into a reaction kettle, the temperature is reduced to room temperature after the hot melt at 200 ℃, and annealing and cleaning volatile auxiliary agents and 40% of polar solvents are added to prepare the dispersion net bag with the dispersion mesh determined as the target mesh for use.
Example 2
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 15 parts of synthetic ester, 7 parts of emulsifier compound, 2 parts of dissolving agent, 15 parts of ethyl acetate, 7 parts of curing agent, 5 parts of organic binder, 10 parts of activated carbon powder, 13 parts of phenol, 20 parts of potassium permanganate solution with the concentration of 0.1mol/l, 8 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
Wherein the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1: 1.5.
Wherein the emulsifier compound comprises polyethylene glycol type nonionic surfactant and anionic surfactant in a ratio of 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
Wherein, the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
Wherein the curing agent is sorbamide.
Wherein the organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
Further, the polar solvent is one or a mixture of more of DPG, PG and DPMA.
Furthermore, 25 parts of hot-melt high-temperature granules and 2 parts of film forming agent are further included, the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive are added into a reaction kettle, the temperature is reduced to room temperature after the hot melt at the temperature of 200 ℃, and annealing and cleaning volatile auxiliary agents and 40% of polar solvents are added to prepare the dispersion net bag with the dispersion mesh determined as the target mesh for use.
Example 3
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 13 parts of synthetic ester, 6 parts of emulsifier compound, 1.5 parts of dissolving agent, 13 parts of ethyl acetate, 6 parts of curing agent, 4 parts of organic binder, 8 parts of activated carbon powder, 12 parts of phenol, 18 parts of potassium permanganate solution with the concentration of 0.1mol/l, 7 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
Wherein the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1: 1.8.
Wherein the emulsifier compound comprises polyethylene glycol type nonionic surfactant and anionic surfactant in a ratio of 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
Wherein, the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
Wherein the curing agent is sodium silicate.
Wherein the organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
Further, the polar solvent is one or a mixture of more of DPG, PG and DPMA.
Furthermore, 23 parts of hot-melt high-temperature granules and 1.5 parts of film forming agent are further included, the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive are added into a reaction kettle, the temperature is reduced to room temperature after the hot melt at the temperature of 200 ℃, and annealing and cleaning volatile auxiliary agents and 40% of polar solvents are added to prepare the dispersion net bag with the dispersion mesh determined as the target mesh for use.
Example 4
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 14 parts of synthetic ester, 5.5 parts of emulsifier compound, 1.8 parts of dissolving agent, 12 parts of ethyl acetate, 5.8 parts of curing agent, 4.2 parts of organic adhesive, 6 parts of activated carbon powder, 11 parts of phenol, 19 parts of potassium permanganate solution with the concentration of 0.1mol/l, 6 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
Wherein the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1: 1.4.
Wherein the emulsifier compound comprises polyethylene glycol type nonionic surfactant and anionic surfactant in a ratio of 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
Wherein, the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
Wherein the curing agent is zinc fluoborate.
Wherein the organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
Further, the polar solvent is one or a mixture of more of DPG, PG and DPMA.
Furthermore, 21 parts of hot-melt high-temperature granules and 1.8 parts of film forming agent are further included, the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive are added into a reaction kettle, the temperature is reduced to room temperature after the hot melt at the temperature of 200 ℃, and annealing and cleaning volatile auxiliary agents and 40% of polar solvents are added to prepare the dispersion net bag with the dispersion mesh determined as the target mesh for use.
Example 5
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 11 parts of synthetic ester, 5.2 parts of emulsifier compound, 1.2 parts of dissolving agent, 12 parts of ethyl acetate, 6.5 parts of curing agent, 3.5 parts of organic adhesive, 9 parts of activated carbon powder, 11 parts of phenol, 18 parts of potassium permanganate solution with the concentration of 0.1mol/l, 7 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
Wherein the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1: 1.8.
Wherein the emulsifier compound comprises polyethylene glycol type nonionic surfactant and anionic surfactant in a ratio of 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
Wherein, the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
Wherein the curing agent is sorbate.
Wherein the organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
Further, the polar solvent is one or a mixture of more of DPG, PG and DPMA.
Furthermore, 23 parts of hot-melt high-temperature granules and 1.7 parts of film forming agent are further included, the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive are added into a reaction kettle, the temperature is reduced to room temperature after the hot melt at the temperature of 200 ℃, the volatile auxiliary agent and 40% of polar solvent are added, and the dispersion net bag with the dispersion mesh determined as the target mesh is manufactured and used.
Example 6
A production and preparation method of an annealing cleaning volatile assistant for aluminum alloy strip rolling oil comprises the following raw materials in parts by weight: 14 parts of synthetic ester, 6.2 parts of emulsifier compound, 1.3 parts of dissolving agent, 15 parts of ethyl acetate, 7 parts of curing agent, 3 parts of organic binder, 6 parts of activated carbon powder, 12 parts of phenol, 17 parts of potassium permanganate solution with the concentration of 0.1mol/l, 5 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and 60% polar solvent into an electrochemical reaction device, slowly dripping potassium permanganate solution at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring at a constant temperature for 3h after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
The synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed according to the ratio of 1: 1.8.
The emulsifier complex comprises polyethylene glycol type nonionic surfactant and anionic surfactant, wherein the weight ratio of the polyethylene glycol type nonionic surfactant to the anionic surfactant is 1: 2, compounding and mixing. The nonionic surfactant is polyoxyethylene amide formed by adding hydroxyl castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
The dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
The curing agent is sodium silicate.
The organic binder comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent. The organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
The polar solvent is one or more of DPG, PG and DPMA.
The preparation method comprises the following steps of adding 22 parts of hot-melt high-temperature granules and 1 part of film forming agent into a reaction kettle, adding the hot-melt high-temperature granules, the film forming agent and 20% of organic adhesive into the reaction kettle, cooling the mixture to room temperature after hot melting at 200 ℃, adding annealing and cleaning volatile auxiliary agents and 40% of polar solvents, and preparing the dispersion net bag with the dispersion mesh determined as the target mesh for use.
Comparative example:
the invention selects a method for preparing rolling oil in the comparative example, which comprises the following steps: the composition comprises the following components in parts by weight:
an oiliness agent: 20 parts of beef tallow and 5 parts of trimethylolpropane oleate;
corrosion inhibitors: 5 parts of petroleum sodium sulfonate, 1 part of fatty acid amide and 4 parts of sodium naphthenate;
emulsifier: 1 part of octyl phenol polyoxyethylene ether and 1.5 parts of fatty alcohol polyoxyethylene ether carboxylic acid;
and (3) a regulator: 1.5 parts of 2- (aminoethoxy) ethanol and 1.5 parts of dicyclohexylamine;
extreme pressure antiwear agent: SLN-1112 parts
Defoaming agent: 0.1 part of organic siloxane copolymer defoaming agent;
base oil: 57.4 parts of refined mineral oil;
additionally adding a volatilization auxiliary agent: as in the above examples 1-6, the conventional common volatile assistant and the non-volatile assistant are added into the comparative sample;
preparation: adding refined mineral oil into a reaction kettle with a stirrer, heating to 40 ℃, starting the stirrer, sequentially adding an oiliness agent, a corrosion inhibitor, an emulsifier, a regulator, an extreme pressure antiwear agent and a defoaming agent, stirring for 90 minutes at a constant temperature until the mixture is clear and transparent, cooling to room temperature, and preparing into rolling oil.
The rolling oil is used for manufacturing the same aluminum alloy plate strip, and the test results are shown in the following table 1:
table 1: table of properties for different cases in comparative examples
Figure BDA0003137671400000111
Figure BDA0003137671400000121
Wherein, the volatilization efficiency is the oil consumption per minute/total oil consumption; the above table shows that the total time of annealing and cleaning and the volatilization efficiency of the invention are far better than those of the volatilization auxiliary agents in the prior art, the surface smoothness of the formed sheet is smoother due to the removal of sulfur element by the attachment of the compound functional group, the oil consumption is only reflected in faster oil consumption rate, but the total oil consumption is reduced due to faster volatilization reaction.
The invention also additionally provides a method for using the volatile agent, which comprises the following steps: adding hot-melt high-temperature granules, a film forming agent and 20% of organic adhesive into a reaction kettle, carrying out hot melting at 200 ℃, cooling to room temperature, adding an annealing and cleaning volatile auxiliary agent and 40% of polar solvent, and preparing into a dispersion net bag with a dispersion mesh as a determined target for use.
The degree of control and the degree of performance in the oil synthesis were carried out by the following methods, as shown in table 2 below:
table 2: rule table for reagent use
Figure BDA0003137671400000122
Figure BDA0003137671400000131
The rolling oil preparation process in the synchronous table 1 adopts the specific parameters in the table 2 to be used after the preparation of the volatilization auxiliary agent when the volatilization efficiency needs to be controlled.
The invention provides a production and preparation method of an annealing cleaning volatilization auxiliary agent for aluminum alloy strip rolling oil, which is prepared by the provided raw materials and a specific process, wherein the performance of the volatilization auxiliary agent is improved by introducing a reflux device and an electrochemical reaction device, the volatilization performance of the volatilization auxiliary agent is essentially improved from a compound, meanwhile, hydroxyl ions are ionized from phenol through electrochemistry, S elements in an aluminum alloy strip can be further removed by integrating other reactants in the annealing process, and the surface performance of a plate is improved.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (10)

1. The production and preparation method of the annealing cleaning volatile assistant for the aluminum alloy strip rolling oil is characterized by comprising the following raw materials in parts by weight: 10-15 parts of synthetic ester, 5-7 parts of emulsifier compound, 1-2 parts of dissolving agent, 10-15 parts of ethyl acetate, 5-7 parts of curing agent, 3-5 parts of organic binder, 5-10 parts of activated carbon powder, 10-13 parts of phenol, 15-20 parts of potassium permanganate solution with the concentration of 0.1mol/l, 5-8 parts of polar solvent and the balance of pure water;
the preparation method of the raw materials comprises the following steps:
s1: quantitative weighing, namely weighing all the raw materials according to the component ratio;
s2: preheating a reaction kettle to 30 ℃, maintaining the temperature within the range of 29-32 ℃, adding a compound of synthetic ester and an emulsifier, slowly dropwise adding a dissolving agent at the speed of 1mol/min, controlling the temperature to 29-32 ℃ after the dissolving agent is completely dropwise added, and stirring for reaction for 30 min;
s3: cooling to an ice point, adding ethyl acetate, maintaining the temperature, stirring for 1h, transferring to an oil bath pan, and configuring a reflux device;
s4: adding a curing agent, 80% of organic binder, activated carbon powder and 20% of water, keeping the reaction kettle sealed, heating the oil bath to 120 ℃, keeping refluxing for 1h after a refluxing phenomenon occurs, and cooling to room temperature;
s5: adding phenol and a 60% polar solvent into an electrochemical reaction device, slowly dripping a potassium permanganate solution into the electrochemical reaction device at the speed of 0.5mol/h after the electrochemical reaction device is externally connected with a 12V power supply, simultaneously monitoring the temperature of a reaction liquid in the electrochemical reaction device in real time, controlling the temperature of the reaction liquid to float upwards by controlling the temperature not to exceed 10 ℃ by adding water, and stirring for 3 hours at a maintained temperature after the potassium permanganate solution is dripped, thus obtaining the annealing cleaning volatilization auxiliary agent.
2. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 1, is characterized in that: the synthetic ester comprises isomeric decanoic acid and isomeric octanoic acid which are compounded and mixed in a ratio of 1:1.4 or 1:1.5 or 1: 1.8.
3. The production and preparation method of the annealing cleaning volatilization auxiliary agent for the aluminum alloy strip rolling oil as set forth in claim 1 or 2, is characterized in that: the emulsifier complex comprises polyethylene glycol type nonionic surfactant and anionic surfactant, wherein the weight ratio of the polyethylene glycol type nonionic surfactant to the anionic surfactant is 1: 2, compounding and mixing.
4. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 3, is characterized in that: the nonionic surfactant is polyoxyethylene amide formed by addition of hydroxyl-containing castor oil and ethylene oxide, and the anionic surfactant is ammonium dodecyl sulfate.
5. The production and preparation method of the annealing cleaning volatilization auxiliary agent for the aluminum alloy strip rolling oil as set forth in claim 1 or 4, is characterized in that: the dissolving agent is one or any two of formic acid, acetonitrile, acetone or butanone in a proportion of 1:1.5 mixing the mixture.
6. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 5, is characterized in that: the curing agent is any one of sorbate, sorbamide, sodium silicate and zinc fluoborate.
7. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 6, is characterized in that: the organic adhesive comprises 10-35 wt% of organic resin and 65-90 wt% of organic solvent.
8. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 7, is characterized in that: the organic resin comprises one or more of acrylic resin, epoxy acrylic resin and dammar resin; the organic solvent comprises two or more of turpentine, PMA, dearomatized solvent oil and dimethyl adipate.
9. The production and preparation method of the annealing cleaning volatile auxiliary for the aluminum alloy strip rolling oil as claimed in claim 1, is characterized in that: the polar solvent is one or a mixture of more of DPG, PG and DPMA.
10. The production and preparation method of the annealing cleaning volatilization auxiliary agent for the aluminum alloy strip rolling oil as set forth in claim 1 or 9, is characterized in that: the preparation method comprises the following steps of adding 20-25 parts of hot-melt high-temperature granules and 1-2 parts of film forming agents into a reaction kettle, adding the hot-melt high-temperature granules, the film forming agents and 20% of organic binders into the reaction kettle, cooling to room temperature after hot melting at 200 ℃, adding the annealing and cleaning volatile auxiliary agents and 40% of polar solvents, and preparing the dispersion net bag with the dispersion mesh determined as the target mesh for use.
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