CN108659929A - A kind of preparation method of oiliness antirust releasing agent - Google Patents

A kind of preparation method of oiliness antirust releasing agent Download PDF

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CN108659929A
CN108659929A CN201810569246.9A CN201810569246A CN108659929A CN 108659929 A CN108659929 A CN 108659929A CN 201810569246 A CN201810569246 A CN 201810569246A CN 108659929 A CN108659929 A CN 108659929A
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releasing agent
antirust
oiliness
obtains
parts
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朱东洋
邓博
陈帅
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/04Mixtures of base-materials and additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/38Treating surfaces of moulds, cores, or mandrels to prevent sticking
    • B28B7/384Treating agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/38Treating surfaces of moulds, cores, or mandrels to prevent sticking
    • B28B7/388Treating surfaces of moulds, cores, or mandrels to prevent sticking with liquid material, e.g. lubricating
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16Paraffin waxes; Petrolatum, e.g. slack wax
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40Fatty vegetable or animal oils
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/12Polysaccharides, e.g. cellulose, biopolymers
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2211/00Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/02Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only
    • C10M2211/024Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only aromatic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22Heterocyclic nitrogen compounds
    • C10M2215/221Six-membered rings containing nitrogen and carbon only
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/041Siloxanes with specific structure containing aliphatic substituents
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/36Release agents or mold release agents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to mold release compositions preparing technical fields, and in particular to a kind of preparation method of oiliness antirust releasing agent.The present invention obtains benevolence slurry by raw material defibrination of gingko benevolence, sodium chloride solution is added into benevolence slurry, cellulase and water obtain benevolence extracting solution, it is ultrasonically treated, it is centrifugally separating to obtain Ginkgo oil, formaldehyde is added into phegma and the mixed liquor of acetophenone obtains parent corrosion inhibiter, parent corrosion inhibiter and benzyl chloride are mixed to get film forming antirust agent, to form a film antirust agent, methenamine, the mixing such as Ginkgo oil, it emulsifies to obtain oiliness antirust releasing agent by high speed dispersion, after oiliness antirust releasing agent is applied to metal surface, it is strong to the barrier absorbability of oxygen in air, and the metal that Ginkgo oil can be aoxidized with part is chelated, improve adhesive force of the oiliness antirust releasing agent to metal, after Mannich base is quaternary ammoniated, after being contacted with metal surface, rotten candle is increased to get rusty the activation energy of reaction, it has a extensive future.

Description

A kind of preparation method of oiliness antirust releasing agent
Technical field
The present invention relates to mold release compositions preparing technical fields, and in particular to a kind of preparation side of oiliness antirust releasing agent Method.
Background technology
Releasing agent is a kind of interface coating being used in the body surface that two are easy to adhesion each other, it can make object table Face be easy to be detached from, it is smooth and clean.Releasing agent not only influences the surface property of composite material, but also whether be related to product can be with It is removed from the mold, either how important product and mold cannot be removed from the mold if fruit product is sticked on mold, Then product and mold can only be scrapped, therefore the effect of releasing agent is of crucial importance.
Good releasing agent should have lubrication and demolding performace good, and cooling and thermal insulation is good, and greasy property is strong, and releasing agent also has There is heat-resisting and stress performance, be not easily decomposed or wear, releasing agent is adhered on mold and is not transfer on processed product, no Interfere spray painting or other secondary machining operations.In addition, releasing agent should not generate pernicious gas and smog, nothing in use It is malicious, safe, easy to operation, cost is more low.
Concrete parting agent type is various both at home and abroad at present, can according to chemical composition be divided into:It is soaps, pure oils, water quality class, molten Agent class, polymerization species, paint class and emulsification oils.Soaps stripping result is general, and aqueous soup solution is alkaline solution, influences to mix Solidifying soil builds surface quality after molding;It is easier to although being demoulded using the pure oils such as machine oil or used oil as release materials, But drying time is longer after coating, and easily stains the clothing and pollution reinforcing bar of constructing operation personnel, and after concrete hardening form removal Also usually there is oil mark on the surface of structures, affects the beauty of concrete surface, and to the later stage ornamental tape of concrete surface Carry out very detrimental effect;Water quality class, which often applies, cannot once be used for multiple times and winter rainy season construction is unavailable;Solvent cost is high Expensive, pollution is big;It is high to polymerize species, paint class cost, clear mould difficulty;Existing emulsification oils releasing agent emulsifying temperature is higher, uses Emulsifier it is more, and the emulsification oil-proofness produced is poor, is susceptible to lamination, is unsuitable for long-term preservation, at Film rear pattern plate rain wash resistance is poor, and the partial emulsifier being on the other hand wherein used in compounding causes serious pollution to the environment, and is unfavorable for big Scale uses.
There are the following problems for releasing agent in the prior art:
(1)It needs that the noxious materials such as toluene or dimethylbenzene are added in preparation process, because it is in releasing agent preparation and application process A large amount of volatilizations, cause pollution of the noxious material to environment, are unfavorable for health and environmental protection, and there are security risks.
A most important raw material is wax in releasing agent, however is with Brazil wax, beeswax etc. in existing releasing agent The wax of foreign countries' production, it is of high cost;Secondly, the wax and fixed oil in releasing agent often settle after placing a period of time, make At uneven inside mould oil, to storage and transportation, using bringing inconvenience.
Stability is poor, and temperature tolerance is relatively low, and service life is short.
Most of wax systems releasing agent using atoleine or lower melting-point microwax due to making it under the high temperature conditions(> 80℃)Stripping result substantially reduce, heat resistance is poor, it is every 1~2 time demoulding after just need to spray again, cause production efficiency big It is big to decline.
For this purpose, being badly in need of inventing a kind of releasing agent and preparation method thereof at low cost, stripping result is good, free from environmental pollution.
Invention content
Present invention mainly solves the technical issues of, for current releasing agent for steel plate demould when, punching block is in high heat condition Lower contacted with air is easily lost, and the defect that steel plate can be also rusted, and provides a kind of system of oiliness antirust releasing agent Preparation Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of oiliness antirust releasing agent, it is characterised in that specifically preparation process is:
(1)It takes 200~250g ginkgo kernels to be put into 30~40min of defibrination in fiberizer, obtains benevolence slurry, benevolence slurry is put Enter in conical flask, 40~50mL sodium chloride solutions, 4~6g cellulases and 200~220mL distilled water be added into conical flask, After enzymolysis, conical flask is placed in water-bath, heat temperature raising is stirred to react, and is filtered, and removal residue collection obtains benevolence extracting solution;
(2)Benevolence extracting solution is placed in sonic oscillation machine, is ultrasonically treated, is obtained sonification fluid, sonification fluid is placed in Centrifugal treating in supercentrifuge, removal lower layer aqueous, it is ginkgo oil that collection, which obtains upper layer oil slick,;
(3)60~70mL aniline and 50~55mL absolute ethyl alcohols are put into the three-necked flask equipped with reflux condenser and blender In, start blender, stirs while 100~120mL hydrochloric acid is added dropwise and flow back back after heating up to three-necked flask heating water bath Flow liquid;
(4)Formaldehyde and acetophenone are mixed, mixed dispersion liquid is obtained, waits for that above-mentioned phegma is cooled to certain temperature, to phegma Middle addition 80~90mL mixed dispersion liquids, are cooled to room temperature, and adjust speed of agitator to 450~480r/min, it is dispersed with stirring 2~ 3h obtains parent corrosion inhibiter;
(5)Parent corrosion inhibiter is mixed with benzyl chloride, obtains mix monomer, to four mouthfuls of burnings equipped with blender and reflux condenser 200~250mL mix monomers, 40~50mL paraffin oils and heat temperature raising are added in bottle, starts blender and stirs, insulation reaction, Obtain film forming antirust agent;
(6)Count in parts by weight, take 70~80 parts film forming antirust agent, 10~12 parts of methenamines, 20~30 parts of Ginkgo oils, 10~ 15 parts of sodium carboxymethylcelluloses, 10~12 parts of methyl silicon resins, 20~25 parts of sorbitan mono fatty acid esters are placed in high speed dispersion In machine, high speed dispersion obtains oiliness antirust releasing agent.
Step(1)The mass fraction of the sodium chloride solution is 15%, and enzymolysis time is 40~45min, after heat temperature raising Temperature is 80~90 DEG C, and it is 40~50min to be stirred to react the time.
Step(2)Temperature is 50~60 DEG C when the described supersound process, and supersonic frequency is 25~30kHz, when supersound process Between be 40~45min, high speed centrifugation rotating speed be 2000~2500r/min, the centrifugal treating time be 15~20min.
Step(3)The mass fraction of the hydrochloric acid is 10%, and temperature is 80~85 after the heating of three-necked flask heating water bath DEG C, return time is 1.0~1.5h.
Step(4)The formaldehyde and acetophenone mixing quality ratio is 1 ︰ 2, and temperature is 60~65 DEG C after phegma cooling.
Step(5)The parent corrosion inhibiter and benzyl chloride mixing quality ratio are 2 ︰ 1, and temperature is 60~65 after heat temperature raising DEG C, the insulation reaction time is 3~4h.
Step(6)The high speed dispersion rotating speed is 3000~3500r/min, and the high speed dispersion time is 10~13min.
The beneficial effects of the invention are as follows:
(1)The present invention obtains benevolence slurry by raw material defibrination of ginkgo nut benevolence, and sodium chloride solution, fibre are added into benevolence slurry The plain enzyme of dimension and water, it is warm that benevolence extracting solution is obtained by the reaction, benevolence extracting solution is ultrasonically treated, is centrifugally separating to obtain ginkgo nut Oil is acidified after mixing aniline with absolute ethyl alcohol, is heated to reflux to obtain phegma, and formaldehyde and acetophenone are added into phegma Mixed liquor is dispersed with stirring to obtain parent corrosion inhibiter, and parent corrosion inhibiter is mixed to get with benzyl chloride by certain mass ratio and mixes list Film forming antirust agent is obtained by the reaction by heating in body, by film forming antirust agent, methenamine, ginkgo nut oil and sodium carboxymethylcellulose Mixing emulsifies to obtain oiliness antirust releasing agent by high speed dispersion, the medium oil antirust releasing agent of the present invention using ginkgo nut oil as Oil phase reduces the macro-molecular protein content in ginkgo nut oil using ultrasonic wave and salting liquid demulsification processing extraction ginkgo nut oil, Make the oxidation stability of oil phase be influenced to reduce by environment acid-base value and temperature, in ginkgo nut oil unsaturated fatty acid content compared with Height, it is strong to the barrier absorbability of oxygen in air after oiliness antirust releasing agent is applied to metal surface, and ginkgo nut oil can be with part The metallic divalent cations aoxidized are chelated, and adhesive force of the oiliness antirust releasing agent to metal is improved, and metal ion can be slowly The unsaturated fatty acid aoxidized is restored, benign cycle is formed, oiliness antirust releasing agent is made to be always maintained at stronger reducing property, To make the rust-proof life of oiliness antirust releasing agent extend;
(2)The parent corrosion inhibiter that the present invention is mixed into oiliness antirust releasing agent is a kind of Mannich base, female after quaternary ammoniated Polar group of the body corrosion inhibiter centered on the larger nitrogen-atoms of electronegativity, polar group hydrophily is very strong, when it is touched After metal surface, there are physisorptions with metal, form adsorption layer, and at the same time, non-polar group is far from metal Direction, form hydrophobicity film, change the state of charge of metal surface, increase rotten candle and get rusty the activation energy of reaction, make rust Change reaction to be difficult to carry out, cation group is carried in parent corrosion inhibiter, to the concentration of metal ions of oiliness antirust releasing agent chelating Have inhibition, can reduction of the catalytic metal ion to saturated fatty acid, make the oil phase unsaturated lipid of oiliness antirust releasing agent Fat acid content is maintained at higher state, and to promote the rustless property of oiliness antirust releasing agent, form a film antirust agent energy and ginkgo nut A small amount of protein combines in oil, and powdery release layer is formed in annealing process, convenient for demoulding, has a extensive future.
Specific implementation mode
It takes 200~250g ginkgo kernels to be put into 30~40min of defibrination in fiberizer, obtains benevolence slurry, by benevolence slurry Be put into conical flask, into conical flask be added 40~50mL mass fractions be 15% sodium chloride solution, 4~6g cellulases and Conical flask is placed in water-bath by 200~220mL distilled water after digesting 40~45min, is heated to 80~90 DEG C, stirring 40~50min is reacted, is filtered, removal residue collection obtains benevolence extracting solution;Benevolence extracting solution is placed in sonic oscillation machine, 40~45min is handled with the frequency ultrasound of 25~30kHz at 50~60 DEG C, sonification fluid is obtained, sonification fluid is placed in Lower layer's aqueous is removed with the rotating speed of 2000~2500r/min, 15~20min of centrifugal treating in supercentrifuge, collection obtains Layer oil slick is ginkgo oil;60~70mL aniline and 50~55mL absolute ethyl alcohols are put into equipped with reflux condenser and blender In three-necked flask, start blender, stirred with the rotating speed of 200~250r/min, while 100~120mL mass fractions are added dropwise and are 10% hydrochloric acid, after being warming up to 80~85 DEG C to three-necked flask heating water bath, flow back 1.0~1.5h, obtains phegma;By formaldehyde It is that 1 ︰ 2 is mixed in mass ratio with acetophenone, mixed dispersion liquid is obtained, when above-mentioned phegma is cooled to 60~65 DEG C, to reflux 80~90mL mixed dispersion liquids are added in liquid, are cooled to room temperature, adjust speed of agitator to 450~480r/min, it is dispersed with stirring 2~ 3h obtains parent corrosion inhibiter;It is that 2 ︰ 1 are mixed in mass ratio by parent corrosion inhibiter and benzyl chloride, obtains mix monomer, to equipped with stirs It mixes and 200~250mL mix monomers, 40~50mL paraffin oils is added in the four-hole boiling flask of device and reflux condenser and is heated to 60~65 DEG C, start blender, stirred with the rotating speed of 300~350r/min, 3~4h of insulation reaction, obtains film forming antirust agent;It presses Parts by weight meter takes 70~80 parts of film forming antirust agent, 10~12 parts of methenamines, 20~30 parts of ginkgo nut oil, 10~15 parts of carboxylics Sodium carboxymethylcellulose pyce, 10~12 parts of methyl silicon resins, 20~25 parts of sorbitan mono fatty acid esters are placed in high speed dispersor, with Rotating speed 10~13min of high speed dispersion of 3000~3500r/min, obtains oiliness antirust releasing agent.
It takes 200g ginkgo kernels to be put into defibrination 30min in fiberizer, obtains benevolence slurry, benevolence slurry is put into conical flask In, sodium chloride solution, 4g cellulases and the 200mL distilled water that 40mL mass fractions are 15%, enzymolysis are added into conical flask After 40min, conical flask is placed in water-bath, is heated to 80 DEG C, is stirred to react 40min, is filtered, removal residue collection obtains To benevolence extracting solution;Benevolence extracting solution is placed in sonic oscillation machine, 40min is handled with the frequency ultrasound of 25kHz at 50 DEG C, Sonification fluid is obtained, sonification fluid is placed in the rotating speed in supercentrifuge with 2000r/min, centrifugal treating 15min is gone Except lower layer's aqueous, it is ginkgo oil that collection, which obtains upper layer oil slick,;60mL aniline and 50mL absolute ethyl alcohols are put into equipped with returned cold In the three-necked flask of condenser and blender, start blender, stirred with the rotating speed of 200r/min, while 100mL mass point is added dropwise Number is 10% hydrochloric acid, and after being warming up to 80 DEG C to three-necked flask heating water bath, flow back 1.0h, obtains phegma;By formaldehyde and benzene second Ketone is that 1 ︰ 2 is mixed in mass ratio, obtains mixed dispersion liquid, when above-mentioned phegma is cooled to 60 DEG C, is added into phegma 80mL mixed dispersion liquids, are cooled to room temperature, and adjust speed of agitator to 450r/min, are dispersed with stirring 2h, obtain parent corrosion inhibiter;It will Parent corrosion inhibiter is that 2 ︰ 1 are mixed in mass ratio with benzyl chloride, mix monomer is obtained, to four equipped with blender and reflux condenser 200mL mix monomers, 40mL paraffin oils are added in mouth flask and is heated to 60 DEG C, startup blender, with turning for 300/min Speed stirring, insulation reaction 3h obtain film forming antirust agent;Count in parts by weight, take 70 parts film forming antirust agent, 10 parts of methenamines, 20 parts of ginkgo nut oil, 10 parts of sodium carboxymethylcelluloses, 10 parts of methyl silicon resins, 20 parts of sorbitan mono fatty acid esters are placed in high speed In dispersion machine, with the rotating speed high speed dispersion 10min of 3000r/min, oiliness antirust releasing agent is obtained.
It takes 225g ginkgo kernels to be put into defibrination 35min in fiberizer, obtains benevolence slurry, benevolence slurry is put into conical flask In, sodium chloride solution, 5g cellulases and the 210mL distilled water that 45mL mass fractions are 15%, enzymolysis are added into conical flask After 43min, conical flask is placed in water-bath, is heated to 85 DEG C, is stirred to react 45min, is filtered, removal residue collection obtains To benevolence extracting solution;Benevolence extracting solution is placed in sonic oscillation machine, 43min is handled with the frequency ultrasound of 27kHz at 55 DEG C, Sonification fluid is obtained, sonification fluid is placed in the rotating speed in supercentrifuge with 2250r/min, centrifugal treating 17min is gone Except lower layer's aqueous, it is ginkgo oil that collection, which obtains upper layer oil slick,;65mL aniline and 53mL absolute ethyl alcohols are put into equipped with returned cold In the three-necked flask of condenser and blender, start blender, stirred with the rotating speed of 225r/min, while 110mL mass point is added dropwise Number is 10% hydrochloric acid, and after being warming up to 83 DEG C to three-necked flask heating water bath, flow back 1.3h, obtains phegma;By formaldehyde and benzene second Ketone is that 1 ︰ 2 is mixed in mass ratio, obtains mixed dispersion liquid, when above-mentioned phegma is cooled to 63 DEG C, is added into phegma 85mL mixed dispersion liquids, are cooled to room temperature, and adjust speed of agitator to 465r/min, are dispersed with stirring 2h, obtain parent corrosion inhibiter;It will Parent corrosion inhibiter is that 2 ︰ 1 are mixed in mass ratio with benzyl chloride, mix monomer is obtained, to four equipped with blender and reflux condenser 225mL mix monomers, 45mL paraffin oils are added in mouth flask and is heated to 63 DEG C, startup blender, with 325r/min's Rotating speed stirs, insulation reaction 3h, obtains film forming antirust agent;It counts in parts by weight, takes 75 parts of film forming antirust agent, 11 parts of Wu Luotuo Product, 25 parts of ginkgo nut oil, 13 parts of sodium carboxymethylcelluloses, 11 parts of methyl silicon resins, 23 parts of sorbitan mono fatty acid esters are placed in In high speed dispersor, with the rotating speed high speed dispersion 12min of 3250r/min, oiliness antirust releasing agent is obtained.
It takes 250g ginkgo kernels to be put into defibrination 40min in fiberizer, obtains benevolence slurry, benevolence slurry is put into conical flask In, sodium chloride solution, 6g cellulases and the 220mL distilled water that 50mL mass fractions are 15%, enzymolysis are added into conical flask After 45min, conical flask is placed in water-bath, is heated to 90 DEG C, is stirred to react 50min, is filtered, removal residue collection obtains To benevolence extracting solution;Benevolence extracting solution is placed in sonic oscillation machine, 45min is handled with the frequency ultrasound of 30kHz at 60 DEG C, Sonification fluid is obtained, sonification fluid is placed in the rotating speed in supercentrifuge with 2500r/min, centrifugal treating 20min is gone Except lower layer's aqueous, it is ginkgo oil that collection, which obtains upper layer oil slick,;70mL aniline and 55mL absolute ethyl alcohols are put into equipped with returned cold In the three-necked flask of condenser and blender, start blender, stirred with the rotating speed of 250r/min, while 120mL mass point is added dropwise Number is 10% hydrochloric acid, and after being warming up to 85 DEG C to three-necked flask heating water bath, flow back 1.5h, obtains phegma;By formaldehyde and benzene second Ketone is that 1 ︰ 2 is mixed in mass ratio, obtains mixed dispersion liquid, when above-mentioned phegma is cooled to 65 DEG C, is added into phegma 90mL mixed dispersion liquids, are cooled to room temperature, and adjust speed of agitator to 480r/min, are dispersed with stirring 3h, obtain parent corrosion inhibiter;It will Parent corrosion inhibiter is that 2 ︰ 1 are mixed in mass ratio with benzyl chloride, mix monomer is obtained, to four equipped with blender and reflux condenser 250mL mix monomers, 50mL paraffin oils are added in mouth flask and is heated to 65 DEG C, startup blender, with 350r/min's Rotating speed stirs, insulation reaction 4h, obtains film forming antirust agent;It counts in parts by weight, takes 80 parts of film forming antirust agent, 12 parts of Wu Luotuo Product, 30 parts of ginkgo nut oil, 15 parts of sodium carboxymethylcelluloses, 12 parts of methyl silicon resins, 25 parts of sorbitan mono fatty acid esters are placed in In high speed dispersor, with the rotating speed high speed dispersion 13min of 3500r/min, oiliness antirust releasing agent is obtained.
The releasing agent that comparative example is produced with company of Wuhan City is as a comparison case
Releasing agent in oiliness antirust releasing agent produced by the present invention and comparative example is detected, testing result is as shown in table 1:
Lubricity is tested
Lubricity uses four-ball tester simulation test, is tested according to SH/T0189.
Erosion test is first sulfuric acid-treated using iron plate, copper sheet is spare as sample through nitric acid treatment, aluminium flake HCl treatment, The releasing agent in oiliness antirust releasing agent produced by the present invention and comparative example is added dropwise in backward above-mentioned sample, and 55 DEG C of constant temperature are placed for 24 hours Observation is taken out afterwards.
Heat-resisting quantity test is by the releasing agent in oiliness antirust releasing agent produced by the present invention and comparative example in 160 DEG C of heating Weight-loss ratio is tested after 4h.
1 performance measurement result of table
From the data in table 1, it can be seen that oiliness antirust releasing agent produced by the present invention, no matter under normal temperature environment or high temperature, high compression ring All there is preferable release property, lubricity and stability, and smaller to the damaging of workpiece and equipment under border, has wide Prospect of the application.

Claims (7)

1. a kind of preparation method of oiliness antirust releasing agent, it is characterised in that specifically preparation process is:
(1)It takes 200~250g ginkgo kernels to be put into 30~40min of defibrination in fiberizer, obtains benevolence slurry, benevolence slurry is put Enter in conical flask, 40~50mL sodium chloride solutions, 4~6g cellulases and 200~220mL distilled water be added into conical flask, After enzymolysis, conical flask is placed in water-bath, heat temperature raising is stirred to react, and is filtered, and removal residue collection obtains benevolence extracting solution;
(2)Benevolence extracting solution is placed in sonic oscillation machine, is ultrasonically treated, is obtained sonification fluid, sonification fluid is placed in Centrifugal treating in supercentrifuge, removal lower layer aqueous, it is ginkgo oil that collection, which obtains upper layer oil slick,;
(3)60~70mL aniline and 50~55mL absolute ethyl alcohols are put into the three-necked flask equipped with reflux condenser and blender In, start blender, stirs while 100~120mL hydrochloric acid is added dropwise and flow back back after heating up to three-necked flask heating water bath Flow liquid;
(4)Formaldehyde and acetophenone are mixed, mixed dispersion liquid is obtained, waits for that above-mentioned phegma is cooled to certain temperature, to phegma Middle addition 80~90mL mixed dispersion liquids, are cooled to room temperature, and adjust speed of agitator to 450~480r/min, it is dispersed with stirring 2~ 3h obtains parent corrosion inhibiter;
(5)Parent corrosion inhibiter is mixed with benzyl chloride, obtains mix monomer, to four mouthfuls of burnings equipped with blender and reflux condenser 200~250mL mix monomers, 40~50mL paraffin oils and heat temperature raising are added in bottle, starts blender and stirs, insulation reaction, Obtain film forming antirust agent;
(6)Count in parts by weight, take 70~80 parts film forming antirust agent, 10~12 parts of methenamines, 20~30 parts of Ginkgo oils, 10~ 15 parts of sodium carboxymethylcelluloses, 10~12 parts of methyl silicon resins, 20~25 parts of sorbitan mono fatty acid esters are placed in high speed dispersion In machine, high speed dispersion obtains oiliness antirust releasing agent.
2. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(1)It is described The mass fraction of sodium chloride solution be 15%, enzymolysis time is 40~45min, and temperature is 80~90 DEG C after heat temperature raising, stirring Reaction time is 40~50min.
3. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(2)It is described Supersound process when temperature be 50~60 DEG C, supersonic frequency be 25~30kHz, sonication treatment time be 40~45min, at a high speed from Heart rotating speed is 2000~2500r/min, and the centrifugal treating time is 15~20min.
4. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(3)It is described Hydrochloric acid mass fraction be 10%, three-necked flask heating water bath heating after temperature be 80~85 DEG C, return time be 1.0~ 1.5h。
5. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(4)It is described Formaldehyde and acetophenone mixing quality ratio be 1 ︰ 2, phegma cooling after temperature be 60~65 DEG C.
6. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(5)It is described Parent corrosion inhibiter and benzyl chloride mixing quality ratio be 2 ︰ 1, temperature is 60~65 DEG C after heat temperature raising, and the insulation reaction time is 3 ~4h.
7. a kind of preparation method of oiliness antirust releasing agent according to claim 1, it is characterised in that:Step(6)It is described High speed dispersion rotating speed be 3000~3500r/min, the high speed dispersion time be 10~13min.
CN201810569246.9A 2018-06-05 2018-06-05 A kind of preparation method of oiliness antirust releasing agent Pending CN108659929A (en)

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