CN109893885A - A kind of weaving preparation method of defoaming agent - Google Patents
A kind of weaving preparation method of defoaming agent Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of weaving defoaming agent, belong to textile industry field.Epoxidised soybean oil is made by raw material of soybean in the present invention, epoxidised soybean oil is dissolved each other with alcohols material in defoaming agent, and open loop occurs in the spinning sizing agent of strong basicity, to reduce bubble outer surface tension, bubble is crushed and is defoamed by outer surface pressure, and defoaming agent is made to be stabilized presence in alkaline environment；Other effective components such as microcrystalline cellulose and silica solution are mixed in the present invention, through filter cake is obtained by filtration, it is with leachy siliceous cellulose gel, soybean oil, amido silicon oil, dehydrated alcohol are aoxidized after soaking methyl-silicone oil, with fumed silica again, isopropanol, the components high speed dispersion such as white carbon black obtain weaving defoaming agent.
Description
Technical field
The invention discloses a kind of preparation methods of weaving defoaming agent, belong to textile industry field.
Background technique
There are nearly 100 classes in whole world textile auxiliary, about 15000 kinds, and 2,800,000 tons of annual output, market sale
Volume is more than 16,000,000,000 dollars, noveltyization, superior, functionalization of the textile auxiliary to textile.China's dyeing in recent years
Rapid development, although for textile auxiliary, China there is also many problems, textile industry is China's weight due to history
The people's livelihood industry wanted, textile auxiliary have a extensive future, and development potentiality is very big.
But these auxiliary agents largely used in textile printing and dyeing industry, such as bleeding agent, refining agent, levelling agent, dispersing agent and solid
The surfactants such as toner, since the conveying of stirring, transmission and liquid material admits air into, to generate a large amount of foam, Jin Erzao
At various failures, negative effect is brought to dyeing quality, seriously affects the quality of product.It was verified that textile printing and dyeing
Answered with defoaming agent: defoaming is rapidly and foam inhibition is lasting, and good dispersion, high temperature resistant, strong acid-base resistance are good with various dyestuff interworking performances,
Not floating oil, without silicon spot, safe and non-toxic, meet environmental requirement, quality is stablized, and suitable viscosity and concentration are easy to use dilution.
In dyeing process, defoaming agent is essential auxiliary agent, according to incompletely statistics, various printing and dyeing needed for China is annual
Auxiliary agent millions of tons, high temperature defoaming agent account for about 1~20,000 tons.But dyeing terylene is especially in dyeing course, due to dyeing
Temperature height (130~140 DEG C), pressure is big (2~4 atmospheric pressure), and alkalinity is strong (pH value 11~14), and general defoaming agent is strong herein
It has been demulsified under alkali, hot conditions, so that the fabric being colored is stained with silicone oil and form silicon spot, cause the immeasurable loss of producer.
Organic silicon defoamer with the advantages that its low surface tension, preferable chemistry and thermal stability, outstanding antifoaming performance by wide
General concern whether has defoaming and suds suppressing properties well in water-based system or nonaqueous systems.But due to its silicon oxygen
Alkane main chain easy fracture and the strong-hydrophobicity of itself in the environment of strong acid-base make it in industries such as biofermentation, copy paper, printing and dyeing
Using being subject to certain restrictions.
As related patent propose Siloxane-Oxyalkylene Copolymers, by polysiloxane backbone with Si-C or Si-O-C key
It is grafted hydrophilic polyether segment, there is certain emulsibility；If patent is by polysiloxane and Siloxane-Oxyalkylene Copolymers
It is used in compounding, further increases the antifoaming performance of lotion.Siloxane-Oxyalkylene Copolymers can be improved organic silicon defoamer and spin
The compatibility in printing and dyeing system is knitted, but still not can solve the problem of siloxanes is easy chain rupture in strong acid alkali systems, in highly basic
It is poor for applicability in system.For another example lotion acid-proof alkaline is improved in relation to a kind of method using starch as stabilizer of patent, still
Since stabilizing agent dosage is larger, so that antifoaming performance is deteriorated.It is to have by mechanical method come dispersing high viscosity there are also patent
Machine silicon composition, high-viscosity organosilicon composition is dispersed in water by the way that highly viscous emulsifier is added, is prepared into organic
Silicon defoaming agent, and patent there are also patent is dropped by the way that low molecular weight polysiloxane is added into high-viscosity organosilicon composition
Its own low viscosity, above-mentioned patent are all that organic silicon defoamer, preparation method are prepared by high-viscosity organosilicon composition
High-viscosity organosilicon composition can be made to be dispersed well, but cannot effectively wrap up high-viscosity organosilicon composition.It is applying
In the dyeing such as cotton, chemical fibre in textile industry, due to use environment harshness, still it is easy to be demulsified, makes high-viscosity organosilicon
Composition aggregation, forms silicon spot, seriously affects the efficiency of dyeing and the quality of final products, cause great damage economically
It loses.
Therefore, inventing a kind of antifoam performance is good under alkali resistance is good and high temperature weaving with defoaming agent is very to textile industry field
It is necessary to.
Summary of the invention
Present invention mainly solves the technical issues of, for current weaving defoaming agent under strong alkali environment defoaming capacity compared with
Difference, slowly, the lower defect of efficiency provides a kind of preparation method of weaving defoaming agent for defoaming agent defoaming under hot conditions.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
It is a kind of weaving with defoaming agent the preparation method comprises the following steps:
Filter cake is put into 4~5h of immersion in methyl-silicone oil, immersion oil cellulose gel is obtained, immersion oil cellulose gel is rushed with acetone
After washing 3~4 times, according to parts by weight, by immersion oil cellulose gel, fumed silica, epoxidised soybean oil, amido silicon oil,
Dehydrated alcohol, isopropanol, emulsifier mixing be placed in high speed disperser with the revolving speed high speed dispersion 10 of 2000~2200r/min~
After 15min, weaving defoaming agent is obtained；
The preparation of epoxidised soybean oil:
(1) 800~1000g soybean is weighed, soybean is placed in crusher after being crushed 40~50min and obtains bean dregs, with 500~
600mL n-hexane impregnates bean dregs, after stirring 30~45min, impregnates 3~4h, filtering removal residue obtains leachate, by leachate
It pours into extraction container, extraction washing 3~5 times washes 400~500mL water every time, obtains contaminated product, contaminated product is placed in evaporation
In device, heat temperature raising evaporates 2~3h, removes distillate, obtains soybean oil；
(2) according to parts by weight, into the four-hole boiling flask for having thermometer, blender, reflux condenser, soybean oil, matter is added
Measure score be 25% formic acid solution, mass fraction be 20% hydrogen peroxide and mass fraction be 65% sulfuric acid, be heated to 80
~85 DEG C, start blender, stirred with the revolving speed of 300~350r/min, obtains reaction product after reacting 2~3h；
(3) above-mentioned reaction product is moved into separatory funnel, stands 3~5min, lower layer's water phase, upper oil phase is separated, with distillation
Water washed reaction product 3~5 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide of mass fraction 40%
Solution adjusts the pH of decontamination product, then is washed with distilled water decontamination product to neutrality, and decontamination product is placed in oil pump
Vacuum distillation obtains epoxidised soybean oil after distilling 40~45min；
The preparation of filter cake:
(1) according to parts by weight, normal heptane, n-butanol and sucrose ester is added to three-necked flask, the silicon for being 25% by mass fraction is molten
Glue, nitric acid solution and the dehydrated alcohol mixing that mass fraction is 5% are added in beaker, stir 15~20min, obtain mixed liquor；
(2) above-mentioned mixed liquor is added dropwise in three-necked flask with constant pressure funnel with the drop rate of 3~5mL/min, simultaneously
Start blender, after stirring 30~45min with 100~120r/min revolving speed, is added dropwise 4~5 to three-necked flask according to parts by weight
Part ammonium hydroxide and the microcrystalline cellulose of 30~40 parts of addition, stand 12~15min, filtering, and removal filtrate obtains filter cake.
Weaving defoaming agent each component raw material, according to parts by weight, including by 40~45 parts of immersion oil cellulose gel, gas phase
30~40 parts of silica, 40~50 parts of epoxidised soybean oil, 10~12 parts of amido silicon oil, 30~40 parts of dehydrated alcohol, isopropyl
20~30 parts of alcohol, 3~5 parts of emulsifier.
Emulsifier is more preferably nonionic surfactant, specially nonylphenol polyoxyethylene ether, octyl phenol polyoxy
Vinethene, lauric acid polyoxyethylene ether, oleic acid polyoxyethylene, sorbitan monostearate, anhydrous sorbitol list oleic acid
Ester, sorbitan trioleate, anhydrous sorbitol monostearate polyoxyethylene ether-ester, loses anhydrous sorbitol tristearate
Water sorbierite list oleic acid polyoxyethylene ester, three stearic acid polyoxyethylene ether ester of anhydrous sorbitol, castor oil polyoxyethylene ether
One or more compounds.
Evaporating temperature in epoxidised soybean oil preparation when contaminated product heat temperature raising is preferably 70~80 DEG C.
Each raw material of reaction product in epoxidised soybean oil preparation, according to parts by weight, including 70~80 parts of soybean oil, quality
The sulphur that 10~12 parts of the hydrogen peroxide and mass fraction that 20~25 parts of the formic acid solution that score is 25%, mass fraction are 20% are 65%
20~30 parts of acid.
The distillation coolant-temperature gage control used of washed reaction product is 50~55 in the specific preparation step of epoxidised soybean oil (3)
DEG C, it is 8.0~8.5 that decontamination product, which adjusts pH,.
In filter cake preparation each raw material according to parts by weight, including 100~110 parts of normal heptane, 4~6 parts of n-butanol and sucrose
0.1~0.3 part of ester, by 10~15 parts of silica solution that mass fraction is 25%, 4~6 parts of the nitric acid solution and nothing that mass fraction is 5%
16~20 parts of water-ethanol.
The mass fraction of ammonium hydroxide is preferably 5% in filter cake preparation, further limit it is added enter microcrystalline cellulose quality be mixing
3~4 times of silica solution quality in liquid.
The beneficial effects of the present invention are:
(1) epoxidised soybean oil is made by raw material of soybean in the present invention, and epoxidised soybean oil is dissolved each other with alcohols material in defoaming agent,
And open loop occurs in the spinning sizing agent of strong basicity, to reduce bubble outer surface tension, bubble is crushed and is disappeared by outer surface pressure
Bubble, above-mentioned ring-opening reaction is reversible reaction related with pH value of solution, and after wash water is complete, pH is reduced, and ring restores, and is made in defoaming agent
Epoxy group can reuse, and defoaming agent, because there are many hydrophilic radicals for band, reaches meeting after a certain concentration in alkaline solution
Form cluster, cluster can will defoaming effective component silicone oil cladding, when encountering strong alkali environment, can will enter the supplied for electronic of cluster from
Son or radical concentration dilution, protect the activity of effective component, so that defoaming agent be made to be stabilized presence in alkaline environment；
(2) other effective components such as microcrystalline cellulose and silica solution are mixed in the present invention, and through filter cake is obtained by filtration, it is band
Leachy siliceous cellulose gel, then after soaking methyl-silicone oil, with fumed silica oxidation soybean oil, amido silicon oil,
Dehydrated alcohol, isopropanol, the components high speed dispersion such as white carbon black obtain weaving defoaming agent, fumed silica large specific surface area,
Density is small, easily disperses, shows hydrophily without hydrophobic treatment, be difficult to infiltrate in organic phase and disperse, but nano-cellulose is solidifying
Methyl-silicone oil can be covered fumed silica by diffusion, subtract fumed silica the adsorbed hydroxyl content in the stomata of glue
Few, aggregation tendency weakens, and surface free energy reduces, and switchs to hydrophobic by hydrophilic, is changed with wellability, the dispersibility of organic phase
It is kind, help to enhance dispersibility of the silicone oil in bubbling system, at high temperature oily phase diffusion rate in nano-cellulose gel
Accelerate, surrounding bubble outer surface, which can reduce, leads to bubbles burst, makes the defoaming rate of methyl-silicone oil under hot conditions in certain journey
Accelerate on degree, while the air hole structure of cellulose is conducive to macrofoam and is changed into vesicle, thus enhance defoaming agent defoaming effect,
It improves efficiency, has a extensive future.
Specific embodiment
800~1000g soybean is weighed, soybean is placed in crusher after being crushed 40~50min and obtains bean dregs, with 500~
600mL n-hexane impregnates bean dregs, after stirring 30~45min, impregnates 3~4h, filtering removal residue obtains leachate, by leachate
It pours into extraction container, extraction washing 3~5 times washes 400~500mL water every time, obtains contaminated product, contaminated product is placed in evaporation
In device, 70~80 DEG C are heated to, evaporates 2~3h, distillate is removed, obtains soybean oil；According to parts by weight, to having
Thermometer, blender, reflux condenser four-hole boiling flask in, 70~80 portions of soybean oils are added, 20~25 parts of mass fractions are 25%
Formic acid solution, 10~12 parts of mass fractions be 20% hydrogen peroxide and 20~30 parts of mass fractions be 65% sulfuric acid, heating rise
Temperature starts blender to 80~85 DEG C, is stirred with the revolving speed of 300~350r/min, obtains reaction product after reacting 2~3h；It will
Above-mentioned reaction product moves into separatory funnel, stands 3~5min, lower layer's water phase, upper oil phase is separated, with 50~55 DEG C of distillation
Water washed reaction product 3~5 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide of mass fraction 40%
The pH that solution adjusts decontamination product is 8.0~8.5, then is washed with distilled water decontamination product to neutrality, by decontamination product
It is placed in oil pump and is evaporated in vacuo, after distilling 40~45min, obtain epoxidised soybean oil, it is spare；According to parts by weight, Xiang Sankou
100~110 portions of normal heptanes, 4~6 parts of n-butanols and 0.1~0.3 part of sucrose ester is added in flask, is by 10~15 parts of mass fractions
25% silica solution, the nitric acid solution and 16~20 parts of dehydrated alcohol mixing that 4~6 parts of mass fractions are 5% are added in beaker, stirring
15~20min obtains mixed liquor；Above-mentioned mixed liquor is added dropwise to three with constant pressure funnel with the drop rate of 3~5mL/min
In mouth flask, while starting blender, after stirring 30~45min with 100~120r/min revolving speed, according to parts by weight to three mouthfuls
Flask is added dropwise the ammonium hydroxide that 4~5 parts of mass fractions are 5% and adds 30~40 parts of microcrystalline cellulose, stands 12~15min, mistake
Filter, removal filtrate obtain filter cake；Above-mentioned filter cake is put into 4~5h of immersion in methyl-silicone oil, immersion oil cellulose gel is obtained, will soak
Oily cellulose gel is with after acetone rinsing 3~4 times, according to parts by weight, by 40~45 parts of immersion oil cellulose gels, 30~40 parts
Fumed silica, 40~50 parts of spare epoxidised soybean oils, 10~12 parts of amido silicon oils, 30~40 parts of dehydrated alcohols, 20~
30 parts of isopropanols, 3~5 parts of emulsifier mixing are placed in the revolving speed high speed dispersion 10 in high speed disperser with 2000~2200r/min
After~15min, weaving defoaming agent is obtained.
Embodiment 1
Emulsifier are as follows: nonylphenol polyoxyethylene ether
The preparation of epoxidised soybean oil:
800g soybean is weighed, soybean is placed in crusher after being crushed 40min and obtains bean dregs, impregnate bean dregs with 500mL n-hexane,
After stirring 30min, 3h is impregnated, filtering removal residue obtains leachate, leachate is poured into extraction container, extraction washing 3 times,
Washing 400mL water every time, obtains contaminated product, contaminated product is placed in vaporising device, is heated to 70 DEG C, evaporates 2h, and removal is steamed
Liquid out obtains soybean oil；
According to parts by weight, into the four-hole boiling flask for having thermometer, blender, reflux condenser, 70 parts of soybean oils, 20 are added
The sulfuric acid that the hydrogen peroxide and 20 parts of mass fractions that formic acid solution that part mass fraction is 25%, 10 parts of mass fractions are 20% are 65%,
80 DEG C are heated to, blender is started, is stirred with the revolving speed of 300r/min, obtains reaction product after reacting 2h；
Above-mentioned reaction product is moved into separatory funnel, 3min is stood, lower layer's water phase, upper oil phase is separated, with 50 DEG C of distillation
Water washed reaction product 3 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide solution of mass fraction 40%
The pH for adjusting decontamination product is 8.0, then is washed with distilled water decontamination product to neutrality, and decontamination product is placed in oil pump
Vacuum distillation obtains epoxidised soybean oil after distilling 40min, spare；
The preparation of filter cake:
According to parts by weight, 100 portions of normal heptanes, 4 parts of n-butanols and 0.1 part of sucrose ester is added to three-necked flask, by 10 parts of quality
The silica solution that score is 25%, the nitric acid solution and 16 parts of dehydrated alcohol mixing that 4 parts of mass fractions are 5% are added in beaker, stirring
15min obtains mixed liquor；Above-mentioned mixed liquor is added dropwise to three-necked flask with constant pressure funnel with the drop rate of 3mL/min
In, while starting blender, after stirring 30min with 100r/min revolving speed, 4 parts of quality are added dropwise to three-necked flask according to parts by weight
The microcrystalline cellulose of 30 parts of ammonium hydroxide and addition that score is 5%, stands 12min, filtering, and removal filtrate obtains filter cake；
The weaving preparation of defoaming agent:
Above-mentioned filter cake is put into methyl-silicone oil and impregnates 4h, obtains immersion oil cellulose gel, by immersion oil cellulose gel acetone
It is according to parts by weight, 40 parts of immersion oil cellulose gels, 30 parts of fumed silicas, 40 parts of spare epoxidations are big after rinsing 3 times
Soya-bean oil, 10 parts of amido silicon oils, 30 parts of dehydrated alcohols, 20 parts of isopropanols, 3 parts of nonylphenol polyoxyethylene ether mixing are placed in high speed dispersion
In machine with the revolving speed high speed dispersion 10min of 2000r/min after, obtain weaving defoaming agent.
Embodiment 2
Emulsifier are as follows: octyl phenol polyoxyethylene ether
The preparation of epoxidised soybean oil:
900g soybean is weighed, soybean is placed in crusher after being crushed 45min and obtains bean dregs, impregnate bean dregs with 550mL n-hexane,
After stirring 37min, 3.5h is impregnated, filtering removal residue obtains leachate, leachate is poured into extraction container, extraction washing 4
Secondary, washing 450mL water, obtains contaminated product, contaminated product is placed in vaporising device every time, is heated to 75 DEG C, evaporates 2.5h, goes
Except distillate, soybean oil is obtained；
According to parts by weight, into the four-hole boiling flask for having thermometer, blender, reflux condenser, 75 parts of soybean oils, 22 are added
The sulfuric acid that the hydrogen peroxide and 25 parts of mass fractions that formic acid solution that part mass fraction is 25%, 11 parts of mass fractions are 20% are 65%,
82 DEG C are heated to, blender is started, is stirred with the revolving speed of 320r/min, obtains reaction product after reacting 2.5h；
Above-mentioned reaction product is moved into separatory funnel, 4min is stood, lower layer's water phase, upper oil phase is separated, with 52 DEG C of distillation
Water washed reaction product 4 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide solution of mass fraction 40%
The pH for adjusting decontamination product is 8.2, then is washed with distilled water decontamination product to neutrality, and decontamination product is placed in oil pump
Vacuum distillation obtains epoxidised soybean oil after distilling 42min, spare；
The preparation of filter cake:
According to parts by weight, 105 portions of normal heptanes, 5 parts of n-butanols and 0.2 part of sucrose ester is added to three-necked flask, by 12 parts of quality
The silica solution that score is 25%, the nitric acid solution and 17 parts of dehydrated alcohol mixing that 5 parts of mass fractions are 5% are added in beaker, stirring
17min obtains mixed liquor；Above-mentioned mixed liquor is added dropwise to three-necked flask with constant pressure funnel with the drop rate of 4mL/min
In, while starting blender, after stirring 40min with 110r/min revolving speed, 4 parts of quality are added dropwise to three-necked flask according to parts by weight
The microcrystalline cellulose of 35 parts of ammonium hydroxide and addition that score is 5%, stands 14min, filtering, and removal filtrate obtains filter cake；
The weaving preparation of defoaming agent:
Above-mentioned filter cake is put into methyl-silicone oil and impregnates 4.5h, obtains immersion oil cellulose gel, by immersion oil cellulose gel with third
After ketone rinses 3 times, according to parts by weight, by 42 parts of immersion oil cellulose gels, 35 parts of fumed silicas, 45 parts of spare epoxidations
Soybean oil, 11 parts of amido silicon oils, 35 parts of dehydrated alcohols, 25 parts of isopropanols, 4 parts of octyl phenol polyoxyethylene ether mixing are placed in high speed point
Dissipate machine in the revolving speed high speed dispersion 12min of 2100r/min after, obtain weaving defoaming agent.
Embodiment 3
Emulsifier are as follows: lauric acid polyoxyethylene ether
The preparation of epoxidised soybean oil:
1000g soybean is weighed, soybean is placed in crusher after being crushed 50min and obtains bean dregs, with 600mL n-hexane soaking beans
Slag after stirring 45min, impregnates 4h, and filtering removal residue obtains leachate, leachate is poured into extraction container, extraction washing 5
Secondary, washing 500mL water, obtains contaminated product, contaminated product is placed in vaporising device every time, is heated to 80 DEG C, evaporates 3h, removal
Distillate obtains soybean oil；
According to parts by weight, into the four-hole boiling flask for having thermometer, blender, reflux condenser, 80 parts of soybean oils, 25 are added
The sulfuric acid that the hydrogen peroxide and 30 parts of mass fractions that formic acid solution that part mass fraction is 25%, 12 parts of mass fractions are 20% are 65%,
85 DEG C are heated to, blender is started, is stirred with the revolving speed of 350r/min, obtains reaction product after reacting 3h；
Above-mentioned reaction product is moved into separatory funnel, 5min is stood, lower layer's water phase, upper oil phase is separated, with 55 DEG C of distillation
Water washed reaction product 5 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide solution of mass fraction 40%
The pH for adjusting decontamination product is 8.5, then is washed with distilled water decontamination product to neutrality, and decontamination product is placed in oil pump
Vacuum distillation obtains epoxidised soybean oil after distilling 45min, spare；
The preparation of filter cake:
According to parts by weight, 110 portions of normal heptanes, 6 parts of n-butanols and 0.3 part of sucrose ester is added to three-necked flask, by 15 parts of quality
The silica solution that score is 25%, the nitric acid solution and 20 parts of dehydrated alcohol mixing that 6 parts of mass fractions are 5% are added in beaker, stirring
20min obtains mixed liquor；Above-mentioned mixed liquor is added dropwise to three-necked flask with constant pressure funnel with the drop rate of 5mL/min
In, while starting blender, after stirring 45min with 120r/min revolving speed, 5 parts of quality are added dropwise to three-necked flask according to parts by weight
The microcrystalline cellulose of 40 parts of ammonium hydroxide and addition that score is 5%, stands 15min, filtering, and removal filtrate obtains filter cake；
The weaving preparation of defoaming agent:
Above-mentioned filter cake is put into methyl-silicone oil and impregnates 5h, obtains immersion oil cellulose gel, by immersion oil cellulose gel acetone
It is according to parts by weight, 45 parts of immersion oil cellulose gels, 40 parts of fumed silicas, 50 parts of spare epoxidations are big after rinsing 4 times
Soya-bean oil, 12 parts of amido silicon oils, 40 parts of dehydrated alcohols, 30 parts of isopropanols, 5 parts of lauric acid polyoxyethylene ether mixing are placed in high speed dispersion
In machine with the revolving speed high speed dispersion 15min of 2200r/min after, obtain weaving defoaming agent.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking epoxidised soybean oil.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking filter cake.
Comparative example 3: the weaving defoaming agent of Shandong company production.
The test of defoaming agent antifoam performance: test equipment: 100mL tool plug graduated cylinder, emperor's balance (precision 0.001g), stopwatch,
Glass beaker, electric furnace, thermometer, glass bar.Test method: shaking flask test: apparatus plug graduated cylinder takes the required standard of 50mL to blister
The defoaming agent sample in Examples 1 to 3 and comparative example is added under 60 DEG C of constant temperatures in medium (5 ‰ ABS aqueous solution)
0.03g covers bottle stopper, and with the frequency of 2 times/second, the amplitude of oscillation of 30~35cm fluctuates graduated cylinder for several times, stands and start timing,
Record foam, which disappears, there is time disappearing the foam inhibition time to get this shaking flask used to liquid level, test result is as follows table 1.
Alkali resistance test: the NaOH aqueous solution of 200mLpH=13 is added in 250mL beaker, adds the embodiment 1 of 4mL
~3 and comparative example in defoaming agent (with concentration be 2% Polyacrylate thickeners aqueous solution 1.19 dilute), be placed on electric furnace
Slowly heating, when liquid level just floccule occurs, writes down the temperature in beaker at this time, the as Precipitation Temperature of the defoaming agent.After
Temperature of continuing rising is cooled to room temperature after boiling 5min, and in observation liquid level state, test result is shown in Table 1.
The test of high temperature defoaming effectiveness: apparatus plug graduated cylinder takes the required standard frothing media (5 ‰ ABS aqueous solution) of 50mL,
Under the conditions of 80 DEG C, the defoaming agent sample 0.03g in Examples 1 to 3 and comparative example is added, covers bottle stopper, with the frequency of 2 times/second,
The amplitude of oscillation of 30~35cm fluctuates graduated cylinder for several times, stands and start timing, and record foam, which disappears, the time used occurs to liquid level, i.e.,
This shaking flask disappears the foam inhibition time, test result is as follows table 1.
Table 1: weaving defoaming agent performance measurement result
Wherein "+" indicates precipitation, and "+" more multilist shows that precipitation is more serious
In summary, weaving of the invention is good with defoaming agent antifoam performance as can be seen from Table 1, and situation is precipitated in alkali system
Few, stability is substantially better than comparative example, while maintaining good antifoam performance, and defoaming capacity is preferable under strong alkali environment,
Defoaming effectiveness under hot environment is high, and foam time is short, with wide with using prospect.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the preparation method that defoaming agent is used in a kind of weaving, it is characterised in that specific preparation step are as follows:
Filter cake is put into 4~5h of immersion in methyl-silicone oil, immersion oil cellulose gel is obtained, immersion oil cellulose gel is rushed with acetone
After washing 3~4 times, according to parts by weight, by immersion oil cellulose gel, fumed silica, epoxidised soybean oil, amido silicon oil,
Dehydrated alcohol, isopropanol, emulsifier mixing be placed in high speed disperser with the revolving speed high speed dispersion 10 of 2000~2200r/min~
After 15min, weaving defoaming agent is obtained；
The specific preparation step of the epoxidised soybean oil are as follows:
(1) 800~1000g soybean is weighed, soybean is placed in crusher after being crushed 40~50min and obtains bean dregs, with 500~
600mL n-hexane impregnates bean dregs, after stirring 30~45min, impregnates 3~4h, filtering removal residue obtains leachate, by leachate
It pours into extraction container, extraction washing 3~5 times washes 400~500mL water every time, obtains contaminated product, contaminated product is placed in evaporation
In device, heat temperature raising evaporates 2~3h, removes distillate, obtains soybean oil；
(2) according to parts by weight, into the four-hole boiling flask for having thermometer, blender, reflux condenser, soybean oil, matter is added
Measure score be 25% formic acid solution, mass fraction be 20% hydrogen peroxide and mass fraction be 65% sulfuric acid, be heated to 80
~85 DEG C, start blender, stirred with the revolving speed of 300~350r/min, obtains reaction product after reacting 2~3h；
(3) above-mentioned reaction product is moved into separatory funnel, stands 3~5min, lower layer's water phase, upper oil phase is separated, with distillation
Water washed reaction product 3~5 times removes lower layer's water phase, upper layer decontamination product is obtained, with the sodium hydroxide of mass fraction 40%
Solution adjusts the pH of decontamination product, then is washed with distilled water decontamination product to neutrality, and decontamination product is placed in oil pump
Vacuum distillation obtains epoxidised soybean oil after distilling 40~45min；
The specific preparation step of the filter cake are as follows:
(1) according to parts by weight, normal heptane, n-butanol and sucrose ester is added to three-necked flask, the silicon for being 25% by mass fraction is molten
Glue, nitric acid solution and the dehydrated alcohol mixing that mass fraction is 5% are added in beaker, stir 15~20min, obtain mixed liquor；
(2) above-mentioned mixed liquor is added dropwise in three-necked flask with constant pressure funnel with the drop rate of 3~5mL/min, simultaneously
Start blender, after stirring 30~45min with 100~120r/min revolving speed, is added dropwise 4~5 to three-necked flask according to parts by weight
Part ammonium hydroxide and the microcrystalline cellulose of 30~40 parts of addition, stand 12~15min, filtering, and removal filtrate obtains filter cake.
2. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the weaving is with disappearing
Infusion each component raw material, according to parts by weight, including by 40~45 parts of immersion oil cellulose gel, fumed silica 30~40
Part, 40~50 parts of epoxidised soybean oil, 10~12 parts of amido silicon oil, 30~40 parts of dehydrated alcohol, 20~30 parts of isopropanol, emulsification
3~5 parts of agent.
3. it is according to claim 1 it is a kind of weaving use defoaming agent preparation method, it is characterised in that: the emulsifier into
One step is preferably nonionic surfactant, specially nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, lauric acid polyoxy
Vinethene, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, anhydrous sorbitol three are hard
Resin acid ester, sorbitan trioleate, anhydrous sorbitol monostearate polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxy
Ethylene ether-ether, three stearic acid polyoxyethylene ether ester of anhydrous sorbitol, castor oil polyoxyethylene ether one or more compounds.
4. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the epoxidation is big
Evaporating temperature in the specific preparation step of soya-bean oil (1) when contaminated product heat temperature raising is preferably 70~80 DEG C.
5. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the epoxidation is big
Each raw material of reaction product in the specific preparation step of soya-bean oil (2), according to parts by weight, including 70~80 parts of soybean oil, mass fraction
For 25% 20~25 parts of formic acid solution, mass fraction be 20% 10~12 parts of hydrogen peroxide and mass fraction be 65% sulfuric acid 20
~30 parts.
6. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the epoxidation is big
The distillation coolant-temperature gage control used of washed reaction product is 50~55 DEG C in the specific preparation step of soya-bean oil (3), and decontamination product is adjusted
PH is 8.0~8.5.
7. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the filter cake is specific
In preparation step (1) each raw material according to parts by weight, including 100~110 parts of normal heptane, 4~6 parts of n-butanol and sucrose ester 0.1
~0.3 part, by 10~15 parts of silica solution that mass fraction is 25%, 4~6 parts of nitric acid solution and anhydrous second that mass fraction is 5%
16~20 parts of alcohol.
8. the preparation method that defoaming agent is used in a kind of weaving according to claim 1, it is characterised in that: the filter cake is specific
The mass fraction of ammonium hydroxide is preferably 5% in preparation step (2), further limit it is added enter microcrystalline cellulose quality be in mixed liquor
3~4 times of silica solution quality.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112057906A (en) * | 2020-08-27 | 2020-12-11 | 江苏赛欧信越消泡剂有限公司 | Low COD defoaming agent for water body without toxicity to microorganisms and preparation method thereof |
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| CN107469413A (en) * | 2017-10-09 | 2017-12-15 | 常州禾吉纺织品有限公司 | A kind of preparation method of alkaline-resisting defoamer |
| CN108126373A (en) * | 2017-12-07 | 2018-06-08 | 常州帝君金属构件厂 | A kind of preparation method of high temperature resistant antifoaming agent |
| CN108909233A (en) * | 2018-05-15 | 2018-11-30 | 谭亚 | A kind of preparation method of nonionic surface active agent fountain solution |
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2019
- 2019-02-28 CN CN201910151391.XA patent/CN109893885A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107469413A (en) * | 2017-10-09 | 2017-12-15 | 常州禾吉纺织品有限公司 | A kind of preparation method of alkaline-resisting defoamer |
| CN108126373A (en) * | 2017-12-07 | 2018-06-08 | 常州帝君金属构件厂 | A kind of preparation method of high temperature resistant antifoaming agent |
| CN108909233A (en) * | 2018-05-15 | 2018-11-30 | 谭亚 | A kind of preparation method of nonionic surface active agent fountain solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112057906A (en) * | 2020-08-27 | 2020-12-11 | 江苏赛欧信越消泡剂有限公司 | Low COD defoaming agent for water body without toxicity to microorganisms and preparation method thereof |
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