CN106046395A - Ternary copolymerized segmented organic silicone oil microemulsion and preparation method and application thereof - Google Patents
Ternary copolymerized segmented organic silicone oil microemulsion and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention provides a ternary copolymerized segmented organic silicone oil microemulsion and a preparation method and application thereof. The ternary polymerized segmented organic silicone oil microemulsion is prepared by weighing ternary copolymerized segmented organic silicone oil; performing stirring at a speed of 700 rpm/min and at a temperature of 30-35 DEG C and adding 1/3 part of a glacial acetic acid aqueous solution; performing stirring for 2 min and adding 1/3 part of the glacial acetic acid aqueous solution and 1/3 part of an emulsifier; performing stirring for 2 min and continuously adding 1/3 part of the glacial acetic acid aqueous solution and 1/3 part of the emulsifier; performing stirring for 2 min and adding the left 1/3 part of the emulsifier; performing stirring for 2 min and increasing the stirring speed; and adding water and performing standing till the obtained product is totally clear. The ternary copolymerized segmented organic silicone oil microemulsion is excellent is acid-base resistance, salt resistance and temperature resistance, can stably cooperate with other additives, and exhibits excellent adsorption to the surface of textile fiber. The emulsion can exhibit excellent stability in a complex working solution environment, and the cost for energy conservation and emission reduction can be saved by 10-30% for a customer.
Description
Technical field
The present invention relates to microemulsion technology field, be specifically related to a kind of terpolymer block organic silicone oil microemulsion and system thereof
Preparation Method.
Background technology
Microemulsion refers to dispersion phase and is uniformly distributed, and particle diameter is less than 200nm, and outward appearance is transparent or translucent ultralow boundary
The Thermodynamically stable emulsion of surface tension.Being compared to common emulsion, microemulsion has the advantages that particle diameter is little, so having good
Wettability and permeability, can penetrate into well and there is fine irregularities grain pattern, the material that small duct and configuration of surface are complicated
In material surface, effect and efficiency for fabric treating all have greatly improved, and the emulsion being simultaneously manufactured has good stablizing
Property, can preserve for a long time and the phenomenon such as breakdown of emulsion, floating oil does not occur.
Silicone oil product active constituent content is the highest and the most water insoluble, so cannot disperse uniformly in water, therefore
Not directly being applicable on fabric, so needing first to be carried out emulsifying, after being made into emulsion, dilution uses.
The character of silicone oil emulsion determines the silicone oil action effect to fabric, therefore, researches and develops silicone oil emulsion of good performance
There is the wide market space.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that one can be prepared has good stability, thoroughly
The method of the terpolymer block organic silicone oil microemulsion that light rate is high.
It is a further object to provide the terpolymer block organic silicone oil microemulsion prepared by said method
Liquid.
It is a further object to provide above-mentioned terpolymer block organic silicone oil microemulsion as chemical & blended fabric
Application in softening agent.
The above-mentioned purpose of the present invention is achieved by following scheme:
The present invention provides the preparation method of a kind of terpolymer block organic silicone oil microemulsion, and this preparation method includes as follows
Step:
Step 1
Glacial acetic acid deionized water is diluted to glacial acetic acid aqueous solution；The quality hundred of glacial acetic acid in described glacial acetic acid aqueous solution
Proportion by subtraction concentration is 50%；
Step 2
Weighing terpolymer block organic silicone oil, open stirring, mixing speed is 700 revs/min, and whipping temp is 30 DEG C
～35 DEG C, add 1/3 part of glacial acetic acid aqueous solution, after stirring 2 minutes, add 1/3 part of glacial acetic acid aqueous solution and 1/3 part of emulsifying agent,
Continuously add 1/3 part of glacial acetic acid aqueous solution and 1/3 part of emulsifying agent after stirring 2 minutes, after stirring 2 minutes, add remaining 1/3 part
Emulsifying agent, after stirring 2 minutes, improves mixing speed to 1200 revs/min～1800 revs/min, adds the most while stirring
Water, stands to clarifying completely after terminating to add water, prepares the terpolymer block organic silicone oil microemulsion of the present invention.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, terpolymer block organic silicone oil uses city
The terpolymer block organic silicone oil sold；Preferred version is that terpolymer block organic silicone oil uses following preparation method to be prepared into
The terpolymer block organic silicone oil arrived:
Allyl glycidyl ether, end containing hydrogen silicone oil and the reaction of allyl glycidyl ether is added in end containing hydrogen silicone oil
Mol ratio is 1:1.05, and limit stirring border ring heats up, and temperature rises to add 3～5ppm platinum catalysts when 90 DEG C, is continuously heating to
110 DEG C are incubated 3～5 hours, prepare end epoxy silicon oil；By end epoxy silicon oil, amine terminated polyether and isopropanol mix homogeneously
After be warming up to 80 DEG C～83 DEG C, keep this temperature reflux react 10 hours, obtain terpolymer block organosilicon crude oil；Add season
Ammonium reagent and terpolymer block silicon crude oil generation quaterisation, then prepare quaterisation product after decompression distillation
Obtain required terpolymer block organic silicone oil.
In the preparation method of above-mentioned terpolymer block organic silicone oil, end containing hydrogen silicone oil use commercially available end containing hydrogen silicone oil or
Person adopts the end containing hydrogen silicone oil prepared with the following method:
1000g octamethylcy-clotetrasiloxane (D4), the hydrogeneous double-seal head of 17.3g and 23g concentrated sulphuric acid are joined four-hole boiling flask
In, temperature controls, at 25 DEG C～40 DEG C, to stir 6～10 hours, be subsequently adding Na2CO3Adjust system pH to pH=7, then through taking out
Filter, blowing prepare end containing hydrogen silicone oil.
In the preparation method of above-mentioned terpolymer block organic silicone oil, allyl glycidyl ether uses commercially available pi-allyl
Glycidyl ether；The amine terminated polyether commercially available molecular weight ranges of employing is the amine terminated polyether of 230～1200.
In the preparation method of above-mentioned terpolymer block organic silicone oil, end epoxy silicon oil and the reaction mole of amine terminated polyether
Ratio is 1:1.2～1:1.5；Isopropanol accounts for the 35%～65% of reactant gross mass；Described reactant gross mass refers to end ring oxygen
The gross mass of silicone oil, amine terminated polyether and isopropanol.
In the preparation method of above-mentioned terpolymer block organic silicone oil, quaternizing agent use benzyl chloride, 2,3-epoxy third
Any one in ammonium chloride, a chloropropane, monochlorethane or dithyl sulfate；Quaternizing agent and terpolymer block silicon
The reaction mol ratio of crude oil is 1:1.1～1:1.25.
In the preparation method of above-mentioned terpolymer block organic silicone oil, the reaction temperature of quaterisation is 80 DEG C～83
DEG C, the response time is 3h～5h；The vacuum of decompression distillation uses-0.08MPa～0.1MPa, decompression distillation to contain to consolidating of product
The distillation procedure that reduces pressure can be stopped when amount is 70%～85%.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, the selection of emulsifying agent is to emulsification extremely
Close important, select suitable emulsifying agent that drop can be made to be uniformly dispersed, the phenomenon of breakdown of emulsion, floating oil will not be produced；The present inventor
By substantial amounts of emulsifying agent is carried out screening and optimizing, finally select by BASF surfactant Lutensol TO5 and emulsifying agent
The emulsifier combination that AEO7 is compounding, in this emulsifier combination, BASF surfactant Lutensol TO5 and emulsifying agent
The mass ratio of AEO7 is 3:7～6:4；Described BASF surfactant Lutensol TO5 uses commercially available prod all can realize this
Invention；Described emulsifying agent AEO7 uses commercially available prod all can realize the present invention.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, total addition of emulsifying agent is ternary polymerization
The 5%～7% of block organic silicone oil gross mass；Total addition of preferred emulsifier is terpolymer block organic silicone oil gross mass
5%；Described emulsifying agent uniformly classifies in three categories part, according to the description in above-mentioned preparation method, is divided into three additions.
Inventor is found by research, and in acid condition, especially pH is about 6 to terpolymer block organic silicone oil
Under the conditions of emulsifying effectiveness the best, and terpolymer block organic silicone oil is alkalescence, can adjust it is contemplated that add which kind of auxiliary agent
Joint system pH can guarantee that again properties of product；By a large amount of conceptual designs and assay optimization, the present invention selects with appropriate glacial acetic acid
Carry out regulation system pH to pH=5.5～6.5, both can guarantee that emulsifying effectiveness well and not interfere with the final performance of product excellent
Good.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, glacial acetic acid uses commercially available technical grade ice vinegar
Acid all can realize the present invention, so that the neutralization of silicone oil system is more abundant, advantageously in forming microemulsion, so glacial acetic acid
It is first to be diluted to, with deionized water, the glacial acetic acid aqueous solution that mass percent concentration is 50%, is the most uniformly divided into three equal parts,
According to the description of above-mentioned preparation method, add in three times；Total addition of described glacial acetic acid aqueous solution is that terpolymer block has
The 1%～3% of machine silicone oil gross mass.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, hydromining deionized water；Adding of water
Enter that amount is terpolymer block organic silicone oil gross weight 3～5 times, preferably 5 times.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, the concrete operations of water while stirring are, first
Mixing speed is adjusted to 1200～1800 revs/min by 700 revs/min, is then kept stirring for speed and is slowly added to water, and
Water is not disposable addition, is uniformly to be divided into 10 equal portions to divide 10 additions, and the time every time added water is 2～3 minutes, then between
Added water after 3～5 minutes, until after adding water for the 10th time all water all being added, standing to clarifying completely the most next time.
In the preparation process of terpolymer block organic silicone oil microemulsion of the present invention, emulsification times preferably 75 minutes, the most just
It is to start stirring from terpolymer block organic silicone oil and emulsifying agent until finally preparing terpolymer block organosilicon
The time of oil Microemulsions For Use.
The present invention also protects the terpolymer block organic silicone oil microemulsion prepared by above-mentioned preparation method, this ternary
Copolymerized block organic silicone oil microemulsion finds through performance test, and it has superior acid and alkali-resistance, salt tolerant and heat resistance, it is possible to
Compatibility stablized by other various auxiliary agents, shows the absorption affinity superior with fabric fibre surface, in complicated working solution environment also
Superior stability can be shown.
The present invention also protects above-mentioned terpolymer block organic silicone oil microemulsion as answering in chemical & blended fabric softening agent
With.
Compared with prior art, there is advantages that
1. the present invention from multiple factors such as emulsifying agent, emulsification system pH value, mixing speed, emulsification times to microemulsion of the present invention
The preparation technology of liquid studies and optimizes, reasonably combined each parameter, selects optimal emulsification condition, thus has obtained stability
Good, light transmittance height, and there is the terpolymer block organic silicone oil microemulsion of blue light；
2. the terpolymer block organic silicone oil microemulsion of the present invention, has superior acid and alkali-resistance, salt tolerant and heat resistance,
Compatibility can be stablized with other various auxiliary agents, show the absorption affinity superior with fabric fibre surface, at complicated work pendular ring
Border also can show superior stability, client can be made to save the cost of 10%～30% at aspects such as energy-conservation, reductions of discharging；
3. the present inventor is found by research, glacial acetic acid is diluted to the glacial acetic acid that mass percent concentration is 50% water-soluble
Liquid uses, and the glacial acetic acid after dilution adds in silicone oil, and the concentration of glacial acetic acid reduces, and it is shallower that the viscosity of silicone oil system increases ratio,
Stirring also becomes to be easy to, and mixing time can also shorten 1/4 accordingly；Meanwhile, acid-base neutralization reaction can slowly be carried out, and makes silicon
It is more abundant that oil systems neutralizes, and is more beneficial for forming microemulsion；
4. the present inventor is found by research, after conventionally disposably being added by emulsifying agent, at least to stir 20
Just minute can obtain uniform silicone oil system, in order to shorten the time, improving emulsifying power and emulsifying effectiveness, the present invention is according to research
Result proposes emulsifying agent is divided into 3 additions, owing to the addition of each emulsifying agent is less, adds latter 2 minutes every time
Stirring, adding for 3 times even if dividing, adding 1 minute of interval, the total time of needs is 9 minutes, also needs than disposable addition
Time shortens 55%, shortens the time, also saves the energy, and advantageously in the formation of microemulsion；
The most traditional emulsion preparation temperature is at about 40 DEG C, and the present invention is arranged in pairs or groups by technique and parameter optimization, especially
3 addition operations of glacial acetic acid aqueous solution and emulsifying agent so that emulsifying temperature can control at 30 DEG C～35 DEG C, advantageously in
Numerical control operating, and save the energy；
6. the preparation technology of the present invention is simple, and each parameter is easy to control, low raw-material cost, and the most large-scale business should
With and promote.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described through, but the present invention is not appointed by specific embodiment
What limits.
The selection of embodiment 1 emulsifying agent
The selection of emulsifying agent is most important to emulsification, selects suitable emulsifying agent that drop can be made to divide equably
Dissipate, the phenomenon of breakdown of emulsion, floating oil will not be produced.
This experiment uses six kinds of emulsifying agents to attempt carrying out emulsifying, and its model is respectively as follows: BASF surfactant
Lutensol XL 30, BASF surfactant Lutensol XL 50, BASF surfactant Lutensol TO5, bar
This husband surfactant Lutensol TO 6, emulsifying agent AEO 3, emulsifying agent AEO 7, result is as shown in table 1.
The impact on emulsifying effectiveness of table 1 emulsifier
According to the result of table 1, TO with AEO series emulsifying agent is used alone and to compound effect preferable.
Again TO Yu AEO series emulsifying agent is used alone and compounds and carry out emulsion light transmittance analysis.
The light transmittance of emulsion refers to that light passes through the luminous flux of emulsion and the percentage ratio of incident flux, and it can be with data
Represent the transparency of emulsion intuitively.
In emulsion light transmittance is analyzed, the emulsion chosen all by the emulsification times fixed, temperature, rotating speed, pH value etc. because of
Element, change factor only has the kind of emulsifying agent, and experimental result is as shown in table 2.
The impact on emulsion transmittance of table 2 emulsifier
By experimental result, the emulsifying agent used that emulsion transmittance is the highest be combined as TO5+AEO7, it is saturating
Light rate is 92.3, and solution appearance is as clear as crystal, and without phenomenons such as floating oils, blue light is sufficient, and the light transmittance of TO6+AEO7 is only second to the former,
But blue light is relatively weak, remaining combination no matter in terms of light transmittance, blue light all not as good as the former, therefore thus can determine that optimum emulsifying
Agent is combined as BASF surfactant Lutensol TO5+ emulsifying agent AEO 7.
The selection of embodiment 2 emulsifier content
Along with the increase of emulsifier, the molecules align between aqueous phase and oil phase interface is tight, so the film formed is strong
Spend higher relative to during low concentration, drop cohesion is caused bigger resistance, thus emulsion intercalation method has the most just obtained phase
The raising answered.So wanting to improve emulsion intercalation method to be accomplished by increasing the usage amount of emulsifying agent, but to consider in the industry
The cost of emulsifying agent, the most in theory, when emulsifier molecules is too much, can form excessive interface energy, the most unfavorable
Stablizing in emulsion.
The present embodiment has carried out series of optimum to emulsifier, and result is as shown in table 3.
The impact on emulsifying effectiveness of table 3 emulsifier content
Note: in table 3, emulsifier content refers to account for the degree of terpolymer block organic silicone oil gross mass
From the experimental result in upper table, when emulsifier is 5%～7%, effect is preferable, rises to 10% left
Time right, blue light has weakened, and illustrates that the particle diameter of emulsion there occurs change, considers emulsifying agent cost, and preferably 5% as emulsifying
The emulsifier of test.
The selection of embodiment 3 emulsification times
Emulsification times has important impact for the final molding of emulsion, if emulsification times is not enough, then silicone oil, water
Not being sufficiently mixed uniformly with emulsifying agent three, can cause emulsion breaking or not emulsified, system is opaque and has cotton-shaped
Thing, or emulsion particle diameter is excessive, makes emulsion unstable.On the contrary, sufficiently stirring can allow emulsion dispersion uniform, particle diameter reduces,
Stability improves, but increases emulsification times simply and can not unrestrictedly improve the quality of emulsion, also can waste simultaneously
Time and resource, increase cost, so selecting an applicable emulsification times critically important to the result of emulsifying.
Emulsification times is optimized by the present embodiment, and result is as shown in table 4.
The impact on emulsifying effectiveness of table 4 emulsification times
| Emulsification times (min) | Emulsion appearance | Stability |
| 25 | Opaque, it is creamy white, has faint blue light | Difference, is placed with layering |
| 45 | Opaque, it is creamy white, blue light is not enough | Poor, there is oil droplet |
| 65 | Close to transparent, having floating thing, blue light is sufficient | Preferably, in stable condition |
| 75 | Close to transparent, without obvious floating thing, blue light is sufficient | Preferably, in stable condition |
| 100 | Close to transparent, without obvious floating thing, blue light is sufficient | Preferably, in stable condition |
According to upper table it is known that when emulsification times was less than 25 minutes, outward appearance and the stability of emulsion are the best, 45 points
Appearance transparent during clock, but there is floating thing, and when 65-100 minute, emulsion has met the requirements from outward appearance and stability, places
After 30 days, emulsion is without layering, the situation of floating oil, and to sum up, preferably 75 minutes as emulsification times.
The selection of embodiment 4 emulsifying pH value
According to pertinent literature, silicone oil is preferably carried out in emulsification in the environment of slant acidity, and Acidity of Aikalinity can
Being adjusted by glacial acetic acid, being suitably added glacial acetic acid can be able to make in emulsion surface formation two-layer with the charged layer of positive charge
Both are mutually exclusive thus be more prone to carry out disperseing and be not easy to be condensed into bigger drop, to emulsifying power and emulsion
Stability all improves a lot, and the less emulsion particle concurrently formed also plays vital work to the molding of microemulsion
With.But too low pH value also can produce impact to the post processing of fabric, make the bursting power of fabric decline, considering cost because of
The reasons such as element and abnormal smells from the patient, are adjusted to about 6 by the pH of emulsion emulsifiers process.Being experimentally confirmed, emulsion is the environment of 6 at pH
In carry out emulsifying, the as clear as crystal not floating oil of emulsion of gained, have abundance blue light, dewatering ability is good, the consumption of glacial acetic acid
Relatively low and abnormal smells from the patient is inconspicuous, to sum up selecting pH is that the environment of 6 is as emulsification condition.
The selection of embodiment 5 mulser rotating speed
Mulser, by the stirring of emulsion is produced shear effect, can make dispersion phase very fast and be evenly distributed in continuously
Xiang Zhong, forms stable emulsion, and mulser is controlled stable at emulsification medium speed, have bright to the final effect of emulsifying
Aobvious raising.
Mulser rotating speed is optimized by the present embodiment, during found that the rotating speed of mulser uses 700r/min, its
Emulsifying effectiveness is good, and emulsion is transparent sufficient blue light, and dewatering ability can be good, and can't produce in emulsion process too much
Foam.
Because after water adds emulsification system, emulsification system can be more and more thicker in emulsion process, so wanting after adding water
Improving rotating speed, inventor, by after data-optimized, selects the rotating speed of 1200～1800 revs/min, is not only able to ensure that stirring is equal
Even, and emulsifying power can be improved.
Embodiment 6 terpolymer block organic silicone oil microemulsion
The terpolymer block organic silicone oil microemulsion of the present embodiment, its preparation method comprises the steps:
Step 1
By 1000g octamethylcy-clotetrasiloxane (D4), the hydrogeneous double-seal head of 17.3g and 23g concentrated sulphuric acid, join with electronic
Blender and the there-necked flask of thermometer, temperature controls, at 30 DEG C～35 DEG C, to stir 6 hours, be subsequently adding Na2CO3Tune system pH
Value is to pH=7, then prepares end containing hydrogen silicone oil through sucking filtration, blowing；Allyl glycidyl ether is added in end containing hydrogen silicone oil,
The reaction mol ratio of end containing hydrogen silicone oil and allyl glycidyl ether is 1:1.05, and limit stirring border ring heats up, and temperature rises to 90
DEG C time add 3～5ppm platinum catalysts, be continuously heating to 110 DEG C be incubated 3～5 hours, prepare end epoxy silicon oil；By end ring
It is warming up to 80 DEG C～83 DEG C after oxygen silicone oil, amine terminated polyether and isopropanol mix homogeneously, keeps this temperature reflux to react 10 hours,
Obtain terpolymer block organosilicon crude oil；Add quaternizing agent and terpolymer block silicon crude oil generation quaterisation,
Quaterisation product is then prepared required terpolymer block organic silicone oil after decompression distillation.
In the preparation method of above-mentioned terpolymer block organic silicone oil, allyl glycidyl ether uses commercially available pi-allyl
Glycidyl ether；The amine terminated polyether commercially available molecular weight ranges of employing is the amine terminated polyether of 230～1200；End epoxy silicon oil and
The reaction mol ratio of amine terminated polyether is 1:1.2；Isopropanol accounts for the 40% of reactant gross mass；Described reactant gross mass refers to
End epoxy silicon oil, amine terminated polyether and the gross mass of isopropanol；Quaternizing agent uses 2,3-glycidyl ammonium chloride；Quaternized
Reagent is 1:1.1 with the reaction mol ratio of terpolymer block silicon crude oil；The reaction temperature of quaterisation is 83 DEG C, during reaction
Between be 3h；The vacuum of decompression distillation uses 0.1MPa, the solid content of decompression distillation to product can stop decompression when being 85%
Distillation procedure.
Step 2
Commercially available BASF surfactant Lutensol TO5 and emulsifying agent AEO7 is configured to according to the mass ratio of 3:7
Emulsifying agent needed for the present embodiment；
Glacial acetic acid deionized water is diluted to the glacial acetic acid aqueous solution that mass percent concentration is 50%；
Step 3
Weighing the terpolymer block organic silicone oil of step 1 preparation, open stirring, mixing speed is 700 revs/min, stirs
Mixing temperature is 30 DEG C～35 DEG C, adds 1/3 part of glacial acetic acid aqueous solution, after stirring 2 minutes, add 1/3 part of glacial acetic acid aqueous solution and
1/3 part of emulsifying agent, continuously adds 1/3 part of glacial acetic acid aqueous solution and 1/3 part of emulsifying agent after stirring 2 minutes, add after stirring 2 minutes
Remaining 1/3 part of emulsifying agent, after stirring 2 minutes, improves mixing speed to 1200 revs/min, keeps this mixing speed to add
Deionized water, deionized water is uniformly to be divided into 10 equal portions to divide 10 additions, and the time every time added water is 2～3 minutes, is then spaced
Add water after 5 minutes the most next time, until after adding water for the 10th time all water all being added, stand to clarification completely and prepare
The terpolymer block organic silicone oil microemulsion of the present embodiment.
In the preparation method of above-mentioned terpolymer block organic silicone oil microemulsion, total addition of emulsifying agent is ternary polymerization
The 5% of block organic silicone oil gross mass；Total addition of glacial acetic acid aqueous solution is terpolymer block organic silicone oil gross mass
3%, total addition of deionized water is 5 times of terpolymer block organic silicone oil gross weight.
The terpolymer block organic silicone oil microemulsion of the present embodiment is carried out performance test, and result is as shown in table 5.
Table 5 emulsion property indices is had a guide look of
As can be seen from Table 5, this terpolymer block organic silicone oil microemulsion has superior acid and alkali-resistance, salt tolerant and heatproof
Performance, can stablize compatibility with other various auxiliary agents, show the absorption affinity superior with fiber surface, therefore in more complicated work
Making also can show in pendular ring border superior stability, light transmittance is high, and this performance can make client save 10 in terms of energy-conservation, reduction of discharging
～the cost of 30%, also provide facility.
Claims (9)
1. the preparation method of a terpolymer block organic silicone oil microemulsion, it is characterised in that this preparation method includes walking as follows
Rapid:
Step 1
Glacial acetic acid deionized water is diluted to the glacial acetic acid aqueous solution that mass percent concentration is 50%；
Step 2
Weighing terpolymer block organic silicone oil, open stirring, mixing speed is 700 revs/min, and whipping temp is 30 DEG C～35
DEG C, add 1/3 part of glacial acetic acid aqueous solution, after stirring 2 minutes, add 1/3 part of glacial acetic acid aqueous solution and 1/3 part of emulsifying agent, stir 2
Continuously add 1/3 part of glacial acetic acid aqueous solution and 1/3 part of emulsifying agent after minute, after stirring 2 minutes, add remaining 1/3 part of emulsifying
Agent, after stirring 2 minutes, improves mixing speed to 1200 revs/min～1800 revs/min, adds water the most while stirring, knot
Stand after Shu Jiashui to clarifying completely, prepare the terpolymer block organic silicone oil microemulsion of the present invention.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
Stating emulsifying agent is emulsifier combination compounding for BASF surfactant Lutensol TO5 and emulsifying agent AEO7.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
The mass ratio stating BASF surfactant Lutensol TO5 and emulsifying agent AEO7 is 3:7～6:4.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
State addition is terpolymer block organic silicone oil gross mass the 5%～7% of emulsifying agent.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
State addition is terpolymer block organic silicone oil gross mass the 1%～3% of glacial acetic acid.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
State water 3～5 times that addition is terpolymer block organic silicone oil gross weight.
The preparation method of a kind of terpolymer block organic silicone oil microemulsion, it is characterised in that institute
Stating water is uniformly to be divided into 10 equal portions to divide 10 additions, and the time every time added water is 2～3 minutes, after being then spaced 3～5 minutes again
Add water next time.
8. a terpolymer block organic silicone oil microemulsion, it is characterised in that this terpolymer block organic silicone oil microemulsion is
It is prepared by the method for any one described in claim 1-7.
9. terpolymer block organic silicone oil microemulsion described in claim 8 is as the application in chemical & blended fabric softening agent.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106592248A (en) * | 2016-12-27 | 2017-04-26 | 清远市宏图助剂有限公司 | Environment-friendly ternary copolymerized segmented organic silicone finishing agent and preparation method thereof |
| CN108498376A (en) * | 2018-04-02 | 2018-09-07 | 榛硕（武汉）智能科技有限公司 | A kind of methyl-silicone oil emulsion and preparation method thereof |
| CN108641097A (en) * | 2018-05-28 | 2018-10-12 | 安徽汇利涂料科技有限公司 | A kind of preparation method of phase inversion waterborne organic silicon lotion |
| CN110004726A (en) * | 2019-05-07 | 2019-07-12 | 纤化（上海）生物化工股份有限公司 | A kind of guarantor's bullet block silicone oil and preparation method thereof for elastic force cowboy |
| CN114232139A (en) * | 2021-12-16 | 2022-03-25 | 连云港神鹰复合材料科技有限公司 | Preparation method of carbon fiber oil for dry-jet wet-spun precursor |
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| 刘瑞云: ""主链聚醚嵌段氨基硅油的合成与应用性能"", 《万方硕士学位论文》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106592248A (en) * | 2016-12-27 | 2017-04-26 | 清远市宏图助剂有限公司 | Environment-friendly ternary copolymerized segmented organic silicone finishing agent and preparation method thereof |
| CN106592248B (en) * | 2016-12-27 | 2019-03-22 | 清远市宏图助剂有限公司 | A kind of environment-friendly type terpolymer block organic silicone finishing agent and preparation method thereof |
| CN108498376A (en) * | 2018-04-02 | 2018-09-07 | 榛硕（武汉）智能科技有限公司 | A kind of methyl-silicone oil emulsion and preparation method thereof |
| CN108641097A (en) * | 2018-05-28 | 2018-10-12 | 安徽汇利涂料科技有限公司 | A kind of preparation method of phase inversion waterborne organic silicon lotion |
| CN110004726A (en) * | 2019-05-07 | 2019-07-12 | 纤化（上海）生物化工股份有限公司 | A kind of guarantor's bullet block silicone oil and preparation method thereof for elastic force cowboy |
| CN110004726B (en) * | 2019-05-07 | 2022-02-08 | 纤化（上海）生物化工股份有限公司 | Elasticity-maintaining block silicone oil for elastic jeans and preparation method thereof |
| CN114232139A (en) * | 2021-12-16 | 2022-03-25 | 连云港神鹰复合材料科技有限公司 | Preparation method of carbon fiber oil for dry-jet wet-spun precursor |
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Application publication date: 20161026 |