CN105839415A - Low-yellowing hydrophilic finishing agent and preparation method thereof - Google Patents
Low-yellowing hydrophilic finishing agent and preparation method thereof Download PDFInfo
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- CN105839415A CN105839415A CN201610242210.0A CN201610242210A CN105839415A CN 105839415 A CN105839415 A CN 105839415A CN 201610242210 A CN201610242210 A CN 201610242210A CN 105839415 A CN105839415 A CN 105839415A
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- D—TEXTILES; PAPER
- 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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- D—TEXTILES; PAPER
- 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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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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
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- D—TEXTILES; PAPER
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- D—TEXTILES; PAPER
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The invention discloses a low-yellowing hydrophilic finishing agent which is characterized by comprising the following components in parts by mass: 100 parts of polysiloxane monomer, 2-13 parts of aminoethyl-aminopropyl-methyldialkoxy silane, 5-40 parts of organic solvent, 1-5 parts of modifier and 5-15 parts of emulsifier. The low-yellowing hydrophilic finishing agent disclosed by the invention has low yellowing, good hydrophilic property and low flow viscosity.
Description
Technical field
The present invention relates to the processing aid of a kind of yarn fabric, a kind of low-yellowing hydrophilic finishing agent and preparation method thereof.
Background technology
Finishing agent is to apply quite varied yarn fabric processing aid at present, and it is mainly added on the surface of yarn fabric, by mutually reciprocal
Should be to reach to give the purpose of yarn fabric specific function.Amino alkyl polysiloxane is the most frequently used yarn fabric finishing agent, its chemistry
Mechanism is to contain amido functional group at the two ends of linear polydimethylsiloxane-.Because its end group is the reactive group that activity is higher, institute
The advantage that flexibility is good, smoothness is high, rub resistance is strong is possessed with amino alkyl polysiloxane.Add extremely using it as finishing agent
During textile surfaces, the excellent flexibility of yarn fabric and good flatness can be given.But, due to amino alkyl polysiloxane
End group be amino, the reactivity of strand two ends group is relatively strong, thus oxidation reaction easily occurs, and causes ammonia alkyl to gather
Organosiloxane has poor chemical stability, the easy breakdown of emulsion of silicone oil emulsion as yarn fabric finishing agent, is easily generated roll banding or floating oil phenomenon
Etc. defect, and after arrangement, silicon speckle easily occurs on fabric.In like manner, the amino group reaction occurred during arranging can cause shallow
The Yellowing that color yarn fabric is expected below in arrangement is fairly obvious, and makes yarn fabric occur serious variable color after arrangement, causes weaving
Color stability extreme difference after thing arrangement.Additionally, the oxidation reaction that amino is during arranging can make natural chemical fiber plus material after arrangement
Hydrophilic extreme difference.
Based on drawbacks described above, yarn fabric processing aid industry occurs in that the modification to amino alkyl polysiloxane, as amidatioon method,
Level Four method etc..But, said method is all just for amino itself, and its reaction mechanism is all by reducing the number of active hydrogen on amino
Amount reduces the reactivity of amino self, to reduce the Yellowing after yarn fabric arranges and to improve its hydrophilic.And said method
Can directly affect the flexibility of amino alkyl polysiloxane self, and the kinematic viscosity of amino alkyl polysiloxane can be significantly increased,
Make its emulsifying the most difficult, thus increase the processing cost of arranging process.Therefore, how to develop one both had reactivity and
Hydrophilic, can reduce again the yarn fabric finishing agent of the Yellowing produced after yarn fabric arranges, be current yarn fabric processing aid industry
One significant technology issues.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of xanthochromia is low, good hydrophilic property and the low use of kinematic viscosity
Low-yellowing hydrophilic finishing agent in yarn fabric processing.
Another object of the present invention is to provide that a kind of technique is simple, reaction stability is strong prepares above-mentioned low-yellowing hydrophilic finishing agent
Method.
The goal of the invention of the present invention is achieved in that a kind of low-yellowing hydrophilic finishing agent, it is characterised in that: described low-yellowing is hydrophilic
Finishing agent includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, organic solvent, modifying agent and emulsifying agent,
Said components is calculated by mass fraction and is respectively as follows: silicone monomers 100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS 2-13
Part;Organic solvent 5-40 part;Modifying agent 1-5 part;Emulsifying agent 5-15 part.
Furtherly, low-yellowing hydrophilic finishing agent also includes basifier, and basifier is figured as 0.05-0.2 part by mass parts.
Optimizing further according to above-mentioned, basifier is that the one in potassium hydroxide or sodium hydroxide or said components are mixed with arbitrary proportion
Close.
Furtherly, low-yellowing hydrophilic finishing agent also includes acidulant, and acidulant is figured as 0.15-0.3 part by mass parts.
Optimizing further according to above-mentioned, acidulant is that the one in acetic acid or propanoic acid or said components mix with arbitrary proportion.
Furtherly, the molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
Wherein R is CH3Or CH2CH3Or CH2CH2CH3Or CH (CH3)2。
Furtherly, one during organic solvent is isopropanol, ethanol, ethylene glycol monobutyl ether, dipropylene glycol or said components are to appoint
Meaning ratio mixes.
Furtherly, one or said components during modifying agent is acrylic acid or ethylene carbonate mix with arbitrary proportion.
Furtherly, emulsifying agent be isomery C13 alcohol ether 5EO, isomery C13 alcohol ether 7EO, branched fatty alcohol-polyoxyethylene ether
One or said components in 7EO, branched fatty alcohol-polyoxyethylene ether 9EO mix with arbitrary proportion.
The present invention also provides for a kind of method preparing above-mentioned low-yellowing hydrophilic finishing agent, and the step of the method is as follows:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 80-110 DEG C while stirring, 50-130 minute response time;
B: add basifier in flask after step a has been reacted, react 3-5 hour at maintaining the temperature at 80-110 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.05-0.1 part acidulant and rear i.e. obtains that ammonia alkyl is poly-to be had
Machine silane;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 50-110 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 10-40 minute in step d gained mixture, after dropping, temperature kept
50-110 DEG C react 1-4 hour, constantly in flask, be filled with nitrogen during reaction, i.e. obtain after having reacted modified amino alkyl gather have
Organic siloxane;
4) preparation of microemulsion:
Lower 20-30 part step e gained mixture of f: normal temperature and pressure and emulsifying agent are placed in flask, and uniformly to stirring;
G: 0.1-0.2 part acidulant is uniformly mixed with the water of 20-30 part, and be slowly added dropwise to f step gained mixture, drip
Add the time 20-50 minute;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5-6 low-yellowing hydrophilic finishing agent.
Furtherly, the viscosity of ammonia alkyl poly-organosilicon alkane is 5000-10000mpa s.
Furtherly, the viscosity of modified amino alkyl polysiloxane is 2000-6000mpa s.
The yarn fabric finishing agent of prior art is improved by the present invention, and its advantage is as follows:
1, in the low-yellowing hydrophilic finishing agent of the present invention, use the active hydrogen displacement reaction of modifying agent and amino, form molecular chain-end
The amino modified system in portion.This modified system can form branched strand group on amino, thus effectively strengthens big point
Sub-chain flexibility, and reduced the viscosity of amino-polysiloxane strand by the improvement of Chain Flexibility, improve finishing agent certainly
The mobility of body.It addition, this modified system can also reduce the active hydrogen quantity on amino, and amino is made to become molecule middle-of-chain
Group, amino is in steady statue in course of reaction all the time, greatly improves the chemical stability of amino-polysiloxane, prevent
There is oxidation reaction in amino during arranging, thus can effectively reduce amino reactivity during arranging, to reduce amino
The polysiloxane xanthochromia when yarn fabric arranges.
2, in the low-yellowing hydrophilic finishing agent of the present invention, silicone monomers and aminoethyl-aminopropyl-methyl dioxane epoxide silicon are used
The hybrid reaction system of alkane.Aminoethyl-aminopropyl-methyl dioxane TMOS self has difunctional reactant group, by with poly-silicon
The reaction of oxygen alkane monomer forms irregular macromolecular chain structure.Further, the reactivity worth of difunctional reactant group is identical, anti-at chemistry
Seasonable as easy as rolling off a log generation molecular isomerism phenomenon, thus thoroughly break the regularity of finishing agent macromolecular chain, except ammonia can be effectively improved
Outside the mobile performance of base polysiloxane, the destruction of strand regularity can also improve yarn fabric flexibility after having arranged
And flatness.
3, in the low-yellowing hydrophilic finishing agent of the present invention, the response type modified system of carboxyl and amino is used.Carboxyl and the contracting of amino
Close reaction and can generate amido link, make amino become the middle group of macromolecular chain, effectively reduce the reactivity of active hydrogen on amino.
On double bond substituted-amino, the modified system of active hydrogen then can be greatly improved the hydrophilicity of finishing agent, thus reduce fibres for fabrics and exist
The water repellent phenomenon occurred after arrangement.
4, in the low-yellowing hydrophilic finishing agent of the present invention, the mixing breast that isomery C13 alcohol ether and fatty alcohol-polyoxyethylene ether are constituted is used
Change system.Isomery C13 alcohol ether and fatty alcohol-polyoxyethylene ether have stronger emulsifying effectiveness, and breast in polysiloxane system
Change effect sufficiently stable.Isomery C13 alcohol ether has excellent permeability, is permeable to fibrous inside, makes fiber surface smooth.
And fatty alcohol-polyoxyethylene ether has good chemical stability, and there is the function improving fiber surface activity, and can be effectively improved
The hydrophilicity of finishing agent.Due to the lifting of emulsifiability, the emulsifying making polysiloxane system is simpler, greatly reduces poly-
The emulsifying difficulty of organosiloxane, reduces the processing cost of arranging process.
5, the low-yellowing hydrophilic finishing agent of the present invention uses alkalization dropping microemulsion method to prepare.First, the reaction environment of alkalization is utilized
Guarantee that silicone monomers and aminoethyl-aminopropyl-methyl dioxane TMOS can fully react, thus ensure silicone monomers with
Molecular isomerism after amino forms strand can be smoothed out.Secondly, amino alkyl polysiloxane drips the same of modifying agent
Time, in chemical reaction environment, constantly it is filled with nitrogen, it is to avoid chemical reaction is played interference effect by the oxygen in air, to ensure chemistry
The stability of reaction and the generation of minimizing side reaction.Finally, modified amino alkyl polysiloxane and the microemulsion of emulsifying agent are utilized
Preparation system, makes the small molecule structure of emulsifying agent can infiltrate in the macromolecular chain structure of amino alkyl polysiloxane smoothly, significantly
Enhance its emulsifying effectiveness.Further, emulsification system adds acidulant, makes the emulsification system tend towards stability, beneficially emulsion reaction
Complete.
Detailed description of the invention
The low-yellowing hydrophilic finishing agent of the present invention includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, organic
Solvent, modifying agent and emulsifying agent, said components is calculated by mass fraction and is respectively as follows: silicone monomers 100 parts;Aminoethyl-aminopropyl
-methyl dioxane TMOS 2-13 part;Organic solvent 5-40 part;Modifying agent 1-5 part;Emulsifying agent 5-15 part.Use poly-silica
Hybrid reaction system on alkane monomer and aminoethyl-aminopropyl-methyl dioxane TMOS strand, and utilize modifying agent and amino
Active hydrogen displacement reaction, improves the Chain Flexibility of amino alkyl polysiloxane, reduces the reactivity of amino, thus carries
The high mobility of amino alkyl polysiloxane, decreases the Yellowing that amino alkyl polysiloxane occurs after arrangement.
In the low-yellowing hydrophilic finishing agent of the present invention, it is also added into basifier.Basifier is figured as 0.05-0.2 part, alkali by mass parts
Agent can use the one in potassium hydroxide or sodium hydroxide or said components to mix with arbitrary proportion.Potassium hydroxide and sodium hydroxide are equal
For highly basic, can provide stable in the chemical reaction process of silicone monomers and aminoethyl-aminopropyl-methyl dioxane TMOS
Alkaline environment, it is ensured that the abundant reaction of aminoethyl-aminopropyl-methyl dioxane TMOS.
In the low-yellowing hydrophilic finishing agent of the present invention, it is also added into acidulant.Acidulant is figured as 0.15-0.3 part, acid by mass parts
Agent is that the one in acetic acid or propanoic acid or said components mix with arbitrary proportion.Acetic acid and propanoic acid are unitary organic monoacid, in acid
In alkali and time will not produce excessively fierce neutralization with alkali and react, the stability of effective guarantee chemical reaction and reliability.
In the low-yellowing hydrophilic finishing agent of the present invention, the molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
Wherein R is CH3Or CH2CH3Or CH2CH2CH3Or CH (CH3)2。
First, R base can be methyl, ethyl, propyl group or isopropyl, and above-mentioned group can form symmetry or asymmetric with siloxy
Property molecular chain structure, thus reduce the regularity of siloxane molecule chain.Secondly, different alkyl is bonded with siloxy, can be real
The isomerization of existing molecular chain structure, can destroy the regularity of siloxane molecule chain equally.
In the low-yellowing hydrophilic finishing agent of the present invention, organic solvent can use isopropanol, ethanol, ethylene glycol monobutyl ether, dipropylene glycol
In one or said components with arbitrary proportion mix.Said components is the most compatible except having between amino alkyl polysiloxane
Outside property, with the mixture of amino alkyl polysiloxane in all with alcohol radical, chemical reaction process can also make whole reaction environment
Relatively alkalescence, the generation of follow-up modified-reaction.
In the low-yellowing hydrophilic finishing agent of the present invention, modifying agent can use the one in acrylic acid or ethylene carbonate or said components with
Arbitrary proportion mixes.Acrylic acid and ethylene carbonate itself carry carboxyl, and its in reaction system in faintly acid, so in alkalescence
Reaction environment under can accelerate and the active hydrogen generation displacement reaction on amino, and generate amido link.This reaction is except effectively reducing
Outside active hydrogen on amino, also make amino presented in intermediate state in amino alkyl polysiloxane, and it is double to introduce carbon-to-carbon
Key.Above-mentioned modified-reaction, in addition to can reducing the reactivity of amino self, also improves the amino chemistry when yarn fabric arranges steady
Qualitative, and improve fiber hydrophilic after arrangement.
In the low-yellowing hydrophilic finishing agent of the present invention, emulsifying agent can use isomery C13 alcohol ether 5EO, isomery C13 alcohol ether 7EO, band
One in the fatty alcohol-polyoxyethylene ether 7EO of chain, branched fatty alcohol-polyoxyethylene ether 9EO or said components are with arbitrary proportion
Mixing.Isomery C13 alcohol ether and fatty alcohol-polyoxyethylene ether have stronger emulsifying effectiveness, and emulsifying in polysiloxane system
Effect is sufficiently stable.And isomery C13 alcohol ether has excellent permeability, fatty alcohol-polyoxyethylene ether then possesses good chemically stable
Property.Fatty alcohol-polyoxyethylene ether uses branched isomer, and it can destroy the rule of polysiloxane strand equally when emulsifying
Whole property, thus reduce the viscosity of polysiloxane.
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 80-110 DEG C while stirring, 50-130 minute response time;
B: add basifier in flask after step a has been reacted, react 3-5 hour at maintaining the temperature at 80-110 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.05-0.1 part acidulant and rear i.e. obtains that ammonia alkyl is poly-to be had
Machine silane;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 50-110 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 10-40 minute in step d gained mixture, after dropping, temperature kept
50-110 DEG C react 1-4 hour, constantly in flask, be filled with nitrogen during reaction, i.e. obtain after having reacted modified amino alkyl gather have
Organic siloxane;
4) preparation of microemulsion:
Lower 20-30 part step e gained mixture of f: normal temperature and pressure and emulsifying agent are placed in flask, and uniformly to stirring;
G: 0.1-0.2 part acidulant is uniformly mixed with the water of 20-30 part, and be slowly added dropwise to f step gained mixture, drip
Add the time 20-50 minute;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5-6 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 5000-10000mpa s, and modified ammonia hydrocarbon
The viscosity of base polysiloxane then can maintain 2000-6000mpa s.Above-mentioned viscosity is that finishing agent strand is in whole reaction system
In mobility characterize, to guarantee that finishing agent adds at yarn fabric and has good mobile performance man-hour.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is
4-5;By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at 6 grams per liters of 100 milliliters
Slightly soluble liquid adds 0.5 gram of sodium carbonate, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention exists
Carrying out constant temperature under this test environment and wave 20 minutes, finishing agent has slight wall built-up-without wall cling phenomenon.By the low Huang to the present invention
Becoming hydrophilic finishing agent and carry out hydrophilic test (testing standard AATCC 79:1995), the average extinction time of water droplet of yarn fabric is 10-70
Second.
It is described in detail below in conjunction with a pair each embodiment of table, but the most therefore limits the invention in described scope of embodiments:
Embodiment 1
The low-yellowing hydrophilic finishing agent of the present invention includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, isopropyl
Alcohol, acrylic acid, isomery C13 alcohol ether 5EO, potassium hydroxide and acetic acid, said components is calculated by mass fraction and is respectively as follows: polysiloxanes
Monomer 100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS 2 parts;Isopropanol 5 parts;1 part of acrylic acid;Isomery C13 alcohol
Ether 5EO 5 parts;Potassium hydroxide 0.05 part;Acetic acid 0.15 part.
The molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 80 DEG C while stirring, 50 minutes response time;
B: add basifier in flask after step a has been reacted, maintains the temperature at and reacts 3 hours at 80 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.05 part of acidulant and i.e. obtains ammonia alkyl poly-organosilicon with rear
Alkane;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 50 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 10 minutes in step d gained mixture, after dropping, temperature be maintained at
50 DEG C are reacted 1 hour, are constantly filled with nitrogen in flask, i.e. obtain modified amino alkyl polysiloxane after having reacted during reaction;
4) preparation of microemulsion:
F: under normal temperature and pressure, 20 parts of step e gained mixture and emulsifying agent are placed in flask, and uniformly to stirring;
G: the water of 0.1 part of acidulant and 20 parts is uniformly mixed, and be slowly added dropwise to f step gained mixture, time for adding
20 minutes;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 10000mpa s, and modified amino alkyl is poly-has
The viscosity of organic siloxane then can maintain 6000mpa s.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is 4;
By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at the slightly soluble liquid of 6 grams per liters of 100 milliliters
0.5 gram of sodium carbonate of middle addition, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention is in this test
Carrying out constant temperature under environment and wave 20 minutes, finishing agent has slight wall cling phenomenon.By the low-yellowing hydrophilic finishing agent of the present invention is entered
Row hydrophilic test (testing standard AATCC 79:1995), the average extinction time of water droplet of yarn fabric is 70 seconds.
Embodiment 2
The low-yellowing hydrophilic finishing agent of the present invention includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, isopropyl
Alcohol, ethanol, ethylene glycol monobutyl ether, dipropylene glycol, acrylic acid, ethylene carbonate, isomery C13 alcohol ether 5EO, isomery C13 alcohol
Ether 7EO, branched fatty alcohol-polyoxyethylene ether 7EO, branched fatty alcohol-polyoxyethylene ether 9EO, potassium hydroxide, hydroxide
Sodium, acetic acid and propanoic acid, said components is calculated by mass fraction and is respectively as follows: silicone monomers 100 parts;Aminoethyl-aminopropyl-methyl
Dialkoxy silicane 13 parts;Isopropanol 10 parts;Ethanol 10 parts;Ethylene glycol monobutyl ether 10 parts;Dipropylene glycol 10 parts;Acrylic acid
3 parts;Ethylene carbonate 2 parts;Isomery C13 alcohol ether 5EO 4 parts;Isomery C13 alcohol ether 7EO 3 parts;Branched poly alkyl alcohol
Oxygen vinyl Ether 7EO 4 parts;Branched fatty alcohol-polyoxyethylene ether 9EO 4 parts;Potassium hydroxide 0.1 part;Sodium hydroxide 0.1 part;
Acetic acid 0.15 part;Propanoic acid 0.15 part.
The molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 110 DEG C while stirring, 130 minutes response time;
B: add basifier in flask after step a has been reacted, maintains the temperature at and reacts 5 hours at 110 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.1 part of acidulant and i.e. obtains ammonia alkyl poly-organosilicon alkane with rear;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 110 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 40 minutes in step d gained mixture, after dropping, temperature be maintained at
110 DEG C are reacted 4 hours, are constantly filled with nitrogen in flask, i.e. obtain modified amino alkyl polysiloxane after having reacted during reaction;
4) preparation of microemulsion:
F: under normal temperature and pressure, 30 parts of step e gained mixture and emulsifying agent are placed in flask, and uniformly to stirring;
G: the water of 0.2 part of acidulant and 30 parts is uniformly mixed, and be slowly added dropwise to f step gained mixture, time for adding
50 minutes;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 6 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 5000mpa s, and modified amino alkyl is poly-has
The viscosity of organic siloxane then can maintain 2000mpa s.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is 4;
By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at the slightly soluble liquid of 6 grams per liters of 100 milliliters
0.5 gram of sodium carbonate of middle addition, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention is in this test
Carrying out constant temperature under environment to wave 20 minutes, finishing agent has without wall cling phenomenon.By the low-yellowing hydrophilic finishing agent of the present invention is carried out
Hydrophilic test (testing standard AATCC 79:1995), the average extinction time of water droplet of yarn fabric is 10 seconds.
Embodiment 3
The low-yellowing hydrophilic finishing agent of the present invention includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, isopropyl
Alcohol, ethanol, dipropylene glycol, ethylene carbonate, isomery C13 alcohol ether 7EO, branched fatty alcohol-polyoxyethylene ether 7EO, band
Fatty alcohol-polyoxyethylene ether 9EO, sodium hydroxide and the propanoic acid of chain, said components is calculated by mass fraction and is respectively as follows: silicone monomers
100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS 4 parts;Isopropanol 5 parts;Ethanol 5 parts;Dipropylene glycol 5 parts;Carbon
Vinyl acetate 2 parts;Isomery C13 alcohol ether 7EO 2 parts;Branched fatty alcohol-polyoxyethylene ether 7EO 3 parts;Branched fat
Polyoxyethylenated alcohol 9EO 3 parts;Sodium hydroxide 0.08 part;Propanoic acid 0.15 part.
The molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 88 DEG C while stirring, 70 minutes response time;
B: add basifier in flask after step a has been reacted, maintains the temperature at and reacts 3.5 hours at 88 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.05 part of acidulant and i.e. obtains ammonia alkyl poly-organosilicon with rear
Alkane;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 65 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 15 minutes in step d gained mixture, after dropping, temperature be maintained at
65 DEG C are reacted 2 hours, are constantly filled with nitrogen in flask, i.e. obtain modified amino alkyl polysiloxane after having reacted during reaction;
4) preparation of microemulsion:
F: under normal temperature and pressure, 23 parts of step e gained mixture and emulsifying agent are placed in flask, and uniformly to stirring;
G: the water of 0.1 part of acidulant and 23 parts is uniformly mixed, and be slowly added dropwise to f step gained mixture, time for adding
30 minutes;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5.2 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 8000mpa s, and modified amino alkyl is poly-has
The viscosity of organic siloxane then can maintain 5000mpa s.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is
4.8;By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at 6 grams per liters of 100 milliliters
Slightly soluble liquid adds 0.5 gram of sodium carbonate, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention exists
Carrying out constant temperature under this test environment and wave 20 minutes, finishing agent has slight wall cling phenomenon.By hydrophilic whole to the low-yellowing of the present invention
Reason agent carries out hydrophilic test (testing standard AATCC 79:1995), and the average extinction time of water droplet of yarn fabric is 60 seconds.
Embodiment 4
The low-yellowing hydrophilic finishing agent of the present invention includes silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, isopropyl
Alcohol, ethylene glycol monobutyl ether, acrylic acid, ethylene carbonate, branched fatty alcohol-polyoxyethylene ether 7EO, branched fatty alcohol
Polyoxyethylene ether 9EO, potassium hydroxide, sodium hydroxide, acetic acid and propanoic acid, said components is calculated by mass fraction and is respectively as follows: poly-silica
Alkane monomer 100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS 7 parts;Isopropanol 10 parts;Ethylene glycol monobutyl ether 10 parts;
2 parts of acrylic acid;Ethylene carbonate 1 part;Branched fatty alcohol-polyoxyethylene ether 7EO 5 parts, branched fatty alcohol polyoxy second
Alkene ether 9EO 6 parts;Potassium hydroxide 0.06 part;Sodium hydroxide 0.06 part;Acetic acid 0.1 part;Propanoic acid 0.1 part.
The molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
Wherein R is CH3Or CH2CH3Or CH2CH2CH3Or CH (CH3)2
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 96 DEG C while stirring, 90 minutes response time;
B: add basifier in flask after step a has been reacted, maintains the temperature at and reacts 4 hours at 96 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.1 part of acidulant and i.e. obtains ammonia alkyl poly-organosilicon alkane with rear;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 85 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 30 minutes in step d gained mixture, after dropping, temperature be maintained at
85 DEG C are reacted 3 hours, are constantly filled with nitrogen in flask, i.e. obtain modified amino alkyl polysiloxane after having reacted during reaction;
4) preparation of microemulsion:
F: under normal temperature and pressure, 26 parts of step e gained mixture and emulsifying agent are placed in flask, and uniformly to stirring;
G: the water of 0.1 part of acidulant and 26 parts is uniformly mixed, and be slowly added dropwise to f step gained mixture, time for adding
40 minutes;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5.5 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 7000mpa s, and modified amino alkyl is poly-has
The viscosity of organic siloxane then can maintain 4000mpa s.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is
4.5;By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at 6 grams per liters of 100 milliliters
Slightly soluble liquid adds 0.5 gram of sodium carbonate, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention exists
Carrying out constant temperature under this test environment to wave 20 minutes, finishing agent has without wall cling phenomenon.By the low-yellowing hydrophilic finiss to the present invention
Agent carries out hydrophilic test (testing standard AATCC 79:1995), and the average extinction time of water droplet of yarn fabric is 40 seconds.
Embodiment 5
The low-yellowing hydrophilic finishing agent of the present invention include silicone monomers, aminoethyl-aminopropyl-methyl dioxane TMOS, ethanol,
Ethylene glycol monobutyl ether, dipropylene glycol, acrylic acid, ethylene carbonate, isomery C13 alcohol ether 5EO, isomery C13 alcohol ether 7EO, band
The fatty alcohol-polyoxyethylene ether 7EO of chain, branched fatty alcohol-polyoxyethylene ether 9EO, potassium hydroxide, sodium hydroxide, acetic acid and third
Acid, said components is calculated by mass fraction and is respectively as follows: silicone monomers 100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS
2-10 part;Ethanol 10 parts;Ethylene glycol monobutyl ether 10 parts;Dipropylene glycol 10 parts;2 parts of acrylic acid;Ethylene carbonate 2 parts;
Isomery C13 alcohol ether 5EO 5 parts;Isomery C13 alcohol ether 7EO 5 parts;Branched fatty alcohol-polyoxyethylene ether 7EO 2 parts, band
The fatty alcohol-polyoxyethylene ether 9EO of chain 2 parts;Potassium hydroxide 0.08 part;Sodium hydroxide 0.08 part;Acetic acid 0.1 part;Propanoic acid 0.15
Part.
The molecular structural formula of aminoethyl-aminopropyl-methyl dioxane TMOS is:
The preparation method of low-yellowing hydrophilic finishing agent of the present invention comprises the steps:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl dioxane oxygen under normal pressure in the flask equipped with agitator and thermometer
Base silane, is heated to 104 DEG C while stirring, 115 minutes response time;
B: add basifier in flask after step a has been reacted, maintains the temperature at and reacts 4 hours at 104 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.1 part of acidulant and i.e. obtains ammonia alkyl poly-organosilicon alkane with rear;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained ammonia hydrocarbon in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Base poly-organosilicon alkane and organic solvent, be heated to 105 DEG C while stirring;
E: be slowly added dropwise modifying agent, time for adding 35 minutes in step d gained mixture, after dropping, temperature be maintained at
105 DEG C are reacted 4 hours, are constantly filled with nitrogen in flask, i.e. obtain modified amino alkyl polysiloxane after having reacted during reaction;
4) preparation of microemulsion:
F: under normal temperature and pressure, 27 parts of step e gained mixture and emulsifying agent are placed in flask, and uniformly to stirring;
G: the water of 0.15 part of acidulant and 28 parts is uniformly mixed, and be slowly added dropwise to f step gained mixture, time for adding
45 minutes;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5.2 low-yellowing hydrophilic finishing agent.
And in whole preparation process, the viscosity of ammonia alkyl poly-organosilicon alkane can maintain 6000mpa s, and modified amino alkyl is poly-has
The viscosity of organic siloxane then can maintain 3000mpa s.
By the low-yellowing hydrophilic finishing agent of the present invention is carried out yellowing-resistant test, (test environment: in yellowing-resistant test box, with 300W
Sample is irradiated 24 hours by bulb, the temperature inside the box constant temperature 50 DEG C), the color inhibition index of the low-yellowing hydrophilic finishing agent of the present invention is 4;
By the low-yellowing hydrophilic finishing agent of the present invention being carried out stability test (test environment: at the slightly soluble liquid of 6 grams per liters of 100 milliliters
0.5 gram of sodium carbonate of middle addition, after agitating solution is uniform, is warming up to 80 DEG C), the low-yellowing hydrophilic finishing agent of the present invention is in this test
Carrying out constant temperature under environment to wave 20 minutes, finishing agent has without wall cling phenomenon.By the low-yellowing hydrophilic finishing agent of the present invention is carried out
Hydrophilic test (testing standard AATCC 79:1995), the average extinction time of water droplet of yarn fabric is 15 seconds.
Table one (in table, component content is mass fraction)
Claims (11)
1. a low-yellowing hydrophilic finishing agent, it is characterised in that: described low-yellowing hydrophilic finishing agent include silicone monomers,
Aminoethyl-aminopropyl-methyl dioxane TMOS, organic solvent, modifying agent and emulsifying agent, said components is figured by mass parts
It is respectively as follows: silicone monomers 100 parts;Aminoethyl-aminopropyl-methyl dioxane TMOS 2-13 part;Organic solvent 5-40
Part;Modifying agent 1-5 part;Emulsifying agent 5-15 part.
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described low-yellowing hydrophilic finishing agent also wraps
Including basifier, basifier is figured as 0.05-0.2 part by mass parts.
Low-yellowing hydrophilic finishing agent the most according to claim 2, it is characterised in that: described basifier is potassium hydroxide or hydrogen
One or said components in sodium oxide mix with arbitrary proportion.
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described low-yellowing hydrophilic finishing agent also wraps
Including acidulant, acidulant is figured as 0.15-0.3 part by mass parts.
Low-yellowing hydrophilic finishing agent the most according to claim 4, it is characterised in that: described acidulant is in acetic acid or propanoic acid
One or said components with arbitrary proportion mix.
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described aminoethyl-aminopropyl-methyl two
The molecular structural formula of alkoxy silane is:
Wherein R is CH3Or CH2CH3Or CH2CH2CH3Or CH (CH3)2。
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described organic solvent is isopropanol, second
One or said components in alcohol, ethylene glycol monobutyl ether, dipropylene glycol mix with arbitrary proportion.
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described modifying agent is acrylic acid or carbonic acid
One or said components in vinyl acetate mix with arbitrary proportion.
Low-yellowing hydrophilic finishing agent the most according to claim 1, it is characterised in that: described emulsifying agent is isomery C13 alcohol ether
5EO, isomery C13 alcohol ether 7EO, branched fatty alcohol-polyoxyethylene ether 7EO, branched fatty alcohol-polyoxyethylene ether 9EO
In one or said components with arbitrary proportion mix.
10. the preparation method of a low-yellowing hydrophilic finishing agent according to claim 1, it is characterised in that: described preparation
The step of method is as follows:
1) corresponding raw material for standby is weighed according to said ratio;
2) preparation of ammonia alkyl poly-organosilicon alkane:
A: add silicone monomers and aminoethyl-aminopropyl-methyl two under normal pressure in the flask equipped with agitator and thermometer
Alkoxy silane, is heated to 80-110 DEG C while stirring, 50-130 minute response time;
B: add basifier in flask after step a has been reacted, react 3-5 hour at maintaining the temperature at 80-110 DEG C;
C: step b gained mixture is naturally cooled to room temperature, adds in 0.05-0.1 part acidulant and i.e. obtains ammonia alkyl with rear
Poly-organosilicon alkane;
3) preparation of modified amino alkyl polysiloxane:
D: add 100 parts of step c gained in the glass flask equipped with agitator, thermometer, reflux and nitrogen charging device
Ammonia alkyl poly-organosilicon alkane and organic solvent, be heated to 50-110 DEG C while stirring;
E: being slowly added dropwise modifying agent in step d gained mixture, time for adding 10-40 minute, temperature after dropping
It is maintained at 50-110 DEG C to react 1-4 hour, constantly in flask, is filled with nitrogen during reaction, after having reacted, i.e. obtains modified ammonia
Alkyl polysiloxane;
4) preparation of microemulsion:
Lower 20-30 part step e gained mixture of f: normal temperature and pressure and emulsifying agent are placed in flask, and uniformly to stirring;
G: 0.1-0.2 part acidulant is uniformly mixed with the water of 20-30 part, and be slowly added dropwise to f step gained mixture,
Time for adding 20-50 minute;
H: in g step gained mixture add water to 100 parts, and pH value be adjusted to 5-6 low-yellowing is hydrophilic whole
Reason agent.
The preparation method of 11. low-yellowing hydrophilic finishing agents according to claim 10, it is characterised in that: described ammonia alkyl gathers
The viscosity of organosilan is 5000-10000mpa s, and the viscosity of described modified amino alkyl polysiloxane is
2000-6000mpa·s。
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CN107724088A (en) * | 2017-10-20 | 2018-02-23 | 广东新翔星科技股份有限公司 | A kind of super hydrophilic low-yellowing silicone softening agent and preparation method thereof |
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