CN110747044B - Biodegradable environment-friendly hydraulic oil and preparation method thereof - Google Patents
Biodegradable environment-friendly hydraulic oil and preparation method thereof Download PDFInfo
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- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
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- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
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- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
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Abstract
The invention provides biodegradable environment-friendly hydraulic oil and a preparation method thereof. The rapeseed oil is cheap and has excellent biodegradability, so that the raw material cost is greatly reduced. The addition of the hawthorn seed oil in the capsule core can improve the oxidation resistance of the rapeseed oil. According to the invention, the rapeseed oil and the hawthorn seed oil are taken as capsule cores to be prepared into microcapsules, and the microcapsule structure can well embed most of the rapeseed oil and the hawthorn seed oil, so that the influence of external conditions is avoided, and the stability of the product is further improved. And finally, mixing the microcapsules with the meadowfoam seed oil and the carnosic acid, wherein the meadowfoam seed oil further plays a role in improving the stability of the rapeseed oil and the hawthorn seed oil which are not embedded by the microcapsules. Carnosic acid is a phenolic acid compound that further enhances the stability of the product.
Description
Technical Field
The invention relates to the technical field of hydraulic oil products, in particular to biodegradable environment-friendly hydraulic oil and a preparation method thereof.
Background
The hydraulic oil is a hydraulic medium used by a hydraulic system utilizing hydraulic pressure energy, and plays roles of energy transfer, abrasion resistance, lubrication, corrosion resistance, rust resistance, cooling and the like in the hydraulic system. The common hydraulic oil in industry is hydrocarbon petroleum, and with the wide use of hydraulic oil, a large amount of hydraulic oil enters the environment in the use process, which causes serious pollution. In order to protect the environment, people pay more and more attention to research and development of biodegradable environment-friendly hydraulic oil in recent years.
The biodegradable hydraulic oil requires that the oil product meets the requirements of the use performance of a hydraulic system, and the self and the consumed product have ecological effects including biodegradability, nontoxicity, renewability and the like. The biodegradable hydraulic oil which is produced or reported at present comprises vegetable oil, ester oil, polyethylene glycol and the like, but is not limited to the vegetable oil or the common synthetic ester hydraulic oil at present. Often contains a large amount of carbon-carbon double bonds, and the oil product has poor oxidation resistance and poor lubricating property, so the oil product is environment-friendly and cannot meet the production requirements.
Patent 104845711B discloses an environment-friendly hydraulic oil, which comprises a component A, a component B and a component C, wherein the component A comprises linseed oil, castor oil, sunflower oil, sorbitan monopalmitate, triglyceride and the like, the component B comprises nano silicon boride, polyalkylene glycol, glycerol, isoparaffin, sulfurized fatty acid ester and the like, the component C comprises trimethylolpropane ester, polyacrylamide, calcium sulfonate, paraffin and the like, and the additive quantity is large, so that the ash content of the hydraulic oil is large, and the biodegradability is poor.
Disclosure of Invention
The invention aims to provide biodegradable environment-friendly hydraulic oil and a preparation method thereof, and the biodegradable environment-friendly hydraulic oil has excellent lubricating property, biodegradability and stability.
In order to achieve the purpose, the invention is realized by the following scheme:
a preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
Preferably, the mass ratio of the rapeseed oil, the hawthorn seed oil, the meadowfoam seed oil and the carnosic acid is 1: 0.06-0.08: 0.2-0.4: 0.08 to 0.1.
Preferably, the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation, extracting for 30 minutes, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder.
Further preferably, the mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
Preferably, the mass concentration of the sodium carboxymethylcellulose aqueous solution is 2-3 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 ℃) for 12-18 hours to obtain the sodium carboxymethylcellulose.
Preferably, the preparation method of the capsule wall solution is as follows: adding starch octenyl succinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring for 2-3 hours at 300-500 rpm.
Preferably, the mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 15-20 g: 100 mL.
Preferably, the mass ratio of the capsule core to the capsule wall solution is 1: 15 to 20.
Preferably, the process conditions of stirring and emulsifying are as follows: stirring for 30-40 minutes at 500-600 rpm.
Preferably, the process conditions of high-pressure homogenization are as follows: homogenizing for 1-2 times under 20-30 MPa, and then homogenizing for 2-3 times under 50-60 MPa.
Preferably, the drying process conditions are as follows: the rotating speed is 16000-22000 r/min, the air inlet speed is 180-200 ℃, the air outlet speed is 80-90 ℃, the feeding temperature is 60-75 ℃, and the feeding speed is 40-50L/h.
Preferably, the process conditions for uniformly mixing the microcapsules, the chinaroot flower seed oil and the carnosic acid are as follows: adding the microcapsule and carnosic acid into the chinaroot flower seed oil, and stirring for 2-3 hours at 200-300 revolutions per minute.
The biodegradable environment-friendly hydraulic oil is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention firstly takes rapeseed oil and hawthorn seed oil as capsule cores to prepare microcapsules, and then the microcapsules are mixed and stirred uniformly with the meadowfoam seed oil and the carnosic acid to obtain the biodegradable environment-friendly hydraulic oil which has excellent lubricating property, biodegradability and stability.
(2) The rapeseed oil is cheap and has excellent biodegradability, so that the raw material cost is greatly reduced. The hawthorn seed oil contains abundant polyphenol compounds, is an excellent donor of hydrogen or electrons, can form a stable phenol free radical intermediate, and has obvious scavenging effect on superoxide anions and hydroxyl free radical energy free radicals which can generate peroxidation to cause structural and functional damage. It shows excellent antioxidant activity due to its high reactivity of hydrogen substitution and its ability to phagocytose free radicals. Therefore, the addition of the hawthorn seed oil in the capsule core can improve the oxidation resistance of the rapeseed oil.
(3) According to the invention, the rapeseed oil and the hawthorn seed oil are taken as capsule cores to be prepared into microcapsules, and the microcapsule structure can well embed most of the rapeseed oil and the hawthorn seed oil, so that the influence of external conditions is avoided, and the stability of the product is further improved.
(4) Finally, the microcapsules are mixed with the meadowfoam seed oil and the carnosic acid, the meadowfoam seed oil contains more than 98 percent of long-chain fatty acid with an antioxidant effect, the long-chain fatty acid cannot be oxidized, and the meadowfoam seed oil further plays a role in improving the stability of the rapeseed oil and the hawthorn seed oil which are not embedded by the microcapsules. Carnosic acid is a phenolic acid compound that further enhances the stability of the product.
(5) As the materials of the microcapsule are basically plant components, have excellent biodegradability and natural lubricity, when the microcapsule is prepared, the octenyl succinic acid starch ester, the oxidized starch and the sodium carboxymethyl cellulose aqueous solution are used for preparing the capsule wall solution, so as to realize the embedding of the capsule core, better embedding can be formed on the capsule core, the oxidation resistance and the stability of the product are improved, and the microcapsule has good biodegradability.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.06: 0.2: 0.08.
the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 2 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 12 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenyl succinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 300 r/min for 2 hr to obtain the final product.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 15 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 15.
the technological conditions of stirring and emulsification are as follows: stirring at 500 rpm for 30 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 20MPa for 1 time, and homogenizing at 50MPa for 2 times.
The drying process conditions are as follows: the rotating speed is 16000 r/min, the air inlet speed is 180 ℃, the air outlet speed is 80 ℃, the feeding temperature is 60 ℃, and the feeding speed is 40L/h.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 200 rpm for 2 hr.
Example 2
A preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.08: 0.4: 0.1.
The preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 3 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 18 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 500 rpm for 3 hr.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 20 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 20.
The technological conditions of stirring and emulsification are as follows: stirring at 600 rpm for 40 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 30MPa for 2 times, and homogenizing at 60MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 22000 r/min, the air inlet speed is 200 ℃, the air outlet speed is 90 ℃, the feeding temperature is 75 ℃, and the feeding speed is 50L/h.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 300 rpm for 3 hr.
Example 3
A preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.06: 0.4: 0.08.
the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation, extracting for 30 minutes, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 3 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 12 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 500 rpm for 2 hr.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 20 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 15.
the process conditions of stirring and emulsifying are as follows: stirring at 600 rpm for 30 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 30MPa for 1 time, and homogenizing at 60MPa for 2 times.
The drying process conditions are as follows: the rotating speed is 22000 r/min, the air inlet speed is 180 ℃, the air outlet speed is 90 ℃, the feeding temperature is 60 ℃ and the feeding speed is 50L/h.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 200 rpm for 3 hr.
Example 4
A preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.08: 0.2: 0.1.
The preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 2 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 18 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 300 rpm for 3 hr.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 15 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 20.
The technological conditions of stirring and emulsification are as follows: stirring at 500 rpm for 40 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 20MPa for 2 times, and homogenizing at 50MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 16000 r/min, the air inlet speed is 200 ℃, the air outlet speed is 80 ℃, the feeding temperature is 75 ℃, and the feeding speed is 40L/h.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 300 rpm for 2 hr.
Example 5
A preparation method of biodegradable environment-friendly hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by using octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.07: 0.3: 0.09.
the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 2.5 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 15 hr to obtain the final product.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 400 rpm for 2 hours to obtain the final product.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 18 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 18.
the technological conditions of stirring and emulsification are as follows: stirring was carried out at 600 rpm for 35 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 25MPa for 1 time, and homogenizing at 55MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 20000 revolutions per minute, the air inlet speed is 190 ℃, the air outlet speed is 85 ℃, the feeding temperature is 70 ℃, and the feeding speed is 45L per hour.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 200 rpm for 3 hr.
Comparative example 1
A preparation method of hydraulic oil comprises the steps of preparing microcapsules by taking rapeseed oil as a capsule core, and then mixing and uniformly stirring the microcapsules, the meadowfoam seed oil and carnosic acid to obtain the biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil to the meadowfoam seed oil to the carnosic acid is 1.07: 0.3: 0.09.
the mass concentration of the sodium carboxymethylcellulose aqueous solution is 2.5 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 15 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 400 rpm for 2 hours to obtain the final product.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 18 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 18.
the technological conditions of stirring and emulsification are as follows: stirring was carried out at 600 rpm for 35 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 25MPa for 1 time, and homogenizing at 55MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 20000 revolutions per minute, the air inlet speed is 190 ℃, the air outlet speed is 85 ℃, the feeding temperature is 70 ℃, and the feeding speed is 45L per hour.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 200 rpm for 3 hr.
Comparative example 2
A preparation method of hydraulic oil comprises the steps of preparing microcapsules by taking rapeseed oil and hawthorn seed oil as capsule cores, and then mixing and stirring the microcapsules and the meadowfoam seed oil uniformly to obtain the biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by utilizing octenyl succinic acid starch ester, oxidized starch and sodium carboxymethyl cellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil to the hawthorn seed oil to the chinaroot flower seed oil is 1: 0.07: 0.39.
the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 2.5 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 15 hr to obtain the final product.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose aqueous solution, and stirring at 400 rpm for 2 hours to obtain the final product.
The mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 18 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 18.
the technological conditions of stirring and emulsification are as follows: stirring was carried out at 600 rpm for 35 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 25MPa for 1 time, and homogenizing at 55MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 20000 revolutions per minute, the air inlet speed is 190 ℃, the air outlet speed is 85 ℃, the feeding temperature is 70 ℃, and the feeding speed is 45L per hour.
The technological conditions for mixing and stirring the microcapsules and the white pond flower seed oil are as follows: the microcapsules were added to meadowfoam seed oil and stirred at 200 rpm for 3 hours.
Comparative example 3
A preparation method of hydraulic oil comprises preparing microcapsule with oleum Rapae and fructus crataegi seed oil as capsule core, mixing microcapsule with Plumbum Preparatium seed oil and carnosic acid, and stirring to obtain biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by using octenyl succinic acid starch ester and a sodium carboxymethylcellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall.
The mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.07: 0.3: 0.09.
the preparation method of the hawthorn seed oil comprises the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation for 30 minutes of extraction, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder. The mass volume ratio of the hawthorn seed powder to the petroleum ether is 1 g: 10 mL.
The mass concentration of the sodium carboxymethylcellulose aqueous solution is 2.5 per mill, and the preparation method comprises the following steps: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature (25 deg.C) for 15 hr.
The preparation method of the capsule wall solution comprises the following steps: adding starch octenylsuccinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring at 400 rpm for 2 hours to obtain the final product.
The mass-volume ratio of the starch octenyl succinate to the sodium carboxymethyl cellulose aqueous solution is 19 g: 100 mL.
The mass ratio of the capsule core solution to the capsule wall solution is 1: 18.
the process conditions of stirring and emulsifying are as follows: stirring was carried out at 600 rpm for 35 minutes.
The process conditions of high-pressure homogenization are as follows: homogenizing at 25MPa for 1 time, and homogenizing at 55MPa for 3 times.
The drying process conditions are as follows: the rotating speed is 20000 revolutions per minute, the air inlet speed is 190 ℃, the air outlet speed is 85 ℃, the feeding temperature is 70 ℃, and the feeding speed is 45L per hour.
The technological conditions for uniformly mixing the microcapsules, the meadowfoam seed oil and the carnosic acid are as follows: adding microcapsule and carnosic acid into white chinaroot flower seed oil, and stirring at 200 rpm for 3 hr.
Test examples
The performance of the hydraulic oils obtained in examples 1 to 5 and comparative examples 1 to 3 was tested, and the results are shown in Table 1.
Wherein the coefficient of friction was measured (50 lbs) using a Ring Block method (Block on Ring) tester (LFW-1) described in ASTM D2174; biodegradability reference CEC L-33-A-93; oxidation stability test referring to ASTM D2893, test oil under specified conditions for air oxidation (121 degrees C, 312 hours), the 100 degrees C kinematic viscosity increase rate, acid value increase and through the microporous filter when the slurry volume; and detecting the initial oxidation temperature of the hydraulic oil.
TABLE 1 Performance test results
As can be seen from Table 1, the hydraulic oils obtained in examples 1 to 5 have good lubricity, stability, oxidation resistance, and excellent biodegradability. In the comparative example 1, rapeseed oil is taken as a capsule core, in the comparative example 2, microcapsules and meadowfoam seed oil are mixed and stirred uniformly to obtain hydraulic oil, in the comparative example 3, octenyl succinic acid starch ester and sodium carboxymethyl cellulose aqueous solution are used for preparing a capsule wall solution, the stability and the oxidation resistance are obviously deteriorated, and the formation of the microcapsule structure and the introduction of hawthorn seed oil in the capsule core and carnosic acid outside the microcapsules are favorable for improving the stability and the oxidation resistance of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A preparation method of biodegradable environment-friendly hydraulic oil is characterized in that firstly rapeseed oil and hawthorn seed oil are taken as capsule cores to prepare microcapsules, and then the microcapsules are mixed and stirred with meadowfoam seed oil and carnosic acid to obtain the biodegradable environment-friendly hydraulic oil; the preparation method of the microcapsule comprises the following steps: preparing a capsule wall solution by using octenyl succinic acid starch ester, oxidized starch and sodium carboxymethylcellulose aqueous solution, then adding a capsule core into the capsule wall solution, stirring and emulsifying, homogenizing under high pressure, and drying to obtain the capsule wall;
the mass ratio of the rapeseed oil, the hawthorn seed oil, the chinaroot flower seed oil and the carnosic acid is 1: 0.06-0.08: 0.2-0.4: 0.08 to 0.1;
the mass-volume ratio of the starch octenyl succinate to the oxidized starch to the sodium carboxymethyl cellulose aqueous solution is 1 g: 15-20 g: 100 mL.
2. The preparation method of claim 1, wherein the hawthorn seed oil is prepared by the following steps: crushing hawthorn seeds, sieving with a 100-mesh sieve to prepare hawthorn seed powder, then taking petroleum ether as an extraction solvent, uniformly mixing the petroleum ether and the hawthorn seed powder, heating and refluxing under 200W ultrasonic oscillation, extracting for 30 minutes, filtering, taking filtrate, and removing the petroleum ether by rotary evaporation to obtain the hawthorn seed powder.
3. The preparation method according to claim 1, wherein the mass concentration of the sodium carboxymethylcellulose aqueous solution is 2-3 ‰, and the preparation method comprises: adding sodium carboxymethylcellulose into water while stirring, and stirring at room temperature for 12-18 hours to obtain the sodium carboxymethylcellulose.
4. The method of claim 1, wherein the wall solution is prepared by the following method: adding starch octenyl succinate and oxidized starch into sodium carboxymethylcellulose water solution, and stirring for 2-3 hours at 300-500 rpm.
5. The preparation method according to claim 1, wherein the mass ratio of the capsule core to the capsule wall solution is 1: 15 to 20.
6. The preparation method according to claim 1, wherein the process conditions of stirring and emulsifying are as follows: stirring for 30-40 minutes at 500-600 rpm.
7. The preparation method according to claim 1, wherein the process conditions of high-pressure homogenization are as follows: homogenizing for 1-2 times under 20-30 MPa, and then homogenizing for 2-3 times under 50-60 MPa.
8. Biodegradable environment-friendly hydraulic oil prepared by the preparation method of any one of claims 1 to 7.
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| BR112013016466B1 (en) * | 2010-12-30 | 2020-05-05 | Union Carbide Chem Plastic | method for manufacturing electrical insulating fluids based on natural ester oil |
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| CN1368842A (en) * | 1998-08-03 | 2002-09-11 | 嘉吉有限公司 | Biodegradable high oxidative stability oils |
| CN105331427A (en) * | 2014-08-11 | 2016-02-17 | 中国石油化工股份有限公司 | Biodegraded plant oil based hydraulic oil composition |
| CN109971535A (en) * | 2019-03-27 | 2019-07-05 | 韩志引 | A kind of coolant liquid and preparation method thereof for hydraulic gear pump |
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