CN102827377A - Amino/sulfydryl co-modified organosilicon polysiloxane microemulsion - Google Patents
Amino/sulfydryl co-modified organosilicon polysiloxane microemulsion Download PDFInfo
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- CN102827377A CN102827377A CN 201210314241 CN201210314241A CN102827377A CN 102827377 A CN102827377 A CN 102827377A CN 201210314241 CN201210314241 CN 201210314241 CN 201210314241 A CN201210314241 A CN 201210314241A CN 102827377 A CN102827377 A CN 102827377A
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- microemulsion
- sulfhydryl
- modified organosilicon
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Abstract
The invention discloses amino/sulfydryl co-modified organosilicon polysiloxane, a synthetic method and a microemulsion composed of amino/sulfydryl co-modified organosilicon polysiloxane, which has a structural formula in the following graph:. The preparation method comprises the following steps: adding hydroxyl-terminated linear silicone oil, a sulfhydryl coupling agent and an amino coupling agent proportionally, stirring and heating, adding a catalyst; stirring and reacting for 1h, controlling the reaction temperature, allowing reaction at a constant temperature for a period, vacuumizing to remove low-molecular substances, and cooling and filtering out insoluble solid with a sieve to obtain the required product; and adding the amino/sulfhydryl co-modified polysiloxane and a certain amount of prepared emulsifying agent to an reactor, then adding amino silicone oil, stirring, sequentially adding phase inversion water and neutralizing acid at the early stage, adding deionized water while stirring to obtain emulsion with 30% solid content, and finally adjusting pH value to about 6 with the neutralizing acid to obtain transparent bluish emulsion. Woolen (cashmere) fabrics treated by the microemulsion feel rich, smooth and soft. to allow reaction for 1h while stirring with reaction temperature controlled, allowing reaction at a constant temperature for a period, vacuumizing to remove low-molecular substances, and cooling and filtering out insoluble solid with a sieve to obtain the required product; and adding the amino/sulfhydryl co-modified polysiloxane and a certain amount of prepared emulsifying agent to an reactor, then adding amino silicone oil, stirring, sequentially adding phase inversion water and neutralizing acid at the early stage, adding deionized water while stirring to obtain emulsion with 30% solid content, and finally adjusting pH value to about 6 with the neutralizing acid to obtain transparent bluish emulsion. Woolen (cashmere) fabrics treated by the microemulsion feel rich, smooth and soft.
Description
(the original bill denomination of invention is: amino/sulfhydryl co-modified organosilicon polysiloxane and compound method thereof and be that December 9, application number in 2008 are 200810177180.5) by its microemulsion that constitutes, the applying date
Technical field
The present invention relates to the microemulsion that a kind of amino/sulfhydryl co-modified organosilicon polysiloxane constitutes.
Background technology
Amino-modified silicone oil has good smooth property, flexibility and film-forming properties, is widely used in the back arrangement processing of multiple textiless such as cotton, silk, wool and terylene.But the structure of different fibers is all inequality with composition, and like wool (suede) fiber, its essentially consist material is the fiber of one type in protein; And the space conformation of protein molecule mainly leans on mainly maintaining like hydrogen bond, sat linkage, disulfide linkage and hydrophobic bond etc. each other between the various groups on main chain and the side chain.According to the woolen chemical constitution, also can find wherein to contain the sulphur of some amount simultaneously.Use softening agent and will prepare the most suitable wool (suede), just must select suitable coupling agents and carry out the copolymerization modification from its woolen chemical constitution and structure.
Summary of the invention
One of the object of the invention is: a kind of amino/sulfhydryl co-modified organosilicon polysiloxane is provided, and structural formula is following:
Wherein: A, B, C are positive integer and A>B >=C;
A=0 ~ 2500; Preferred A=100 ~ 1600;
B=0 ~ 80; Preferred B=10 ~ 60;
C=0 ~ 50; Preferred C=5 ~ 20;
R is-OH ,-CH
3,-OCH
3
R
1For-C
3H
6NHC
2H
4NH
2Or-C
3H
6NHC
3H
6N (CH
3)
2
R
2For-SC
3H
6Si (OCH
3)
2CH
3Or-SC
3H
6Si (OC
2H
5)
2CH
3
Two of the object of the invention is: the preparation method that above-mentioned amino/sulfhydryl co-modified organosilicon polysiloxane is provided.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
Drop into hydroxy-end capped linear silicone oils by a certain percentage, add sulfydryl coupling agent and amino coupling agent mixtinite, stir and be warming up to 85 ~ 90 ℃; Add catalyzer, behind the stirring reaction 1h, control reaction temperature is at 105 ~ 110 ℃; Insulation reaction 5h ~ 8h vacuumizes, and deviates from lower-molecular substance; The cooling back leaches solid insoluble with filter screen, obtains water white amino/sulfhydryl co-modified organosilicon polysiloxane;
Described hydroxy-end capped linear silicone oils, nonvolatile substances content>=99.5%, water cut≤0.1%, viscosity is at (20 ~ 120) mPa.S, and consumption is 60% ~ 85% of hydroxy-end capped linear silicone oils, sulfydryl coupling agent and an amino coupling agent gross weight.
The structure of described sulfydryl coupling agent can be SHC shown in R2
3H
6Si (OCH
3)
2CH
3Or SHC
3H
6Si (OC
2H
5)
2CH
3, consumption is through 2 ~ 20% of basic end-blocking linear silicone oils, coloured glaze base coupling agent and amino coupling agent gross weight;
The structure of amino coupling agent can be-C shown in R1
3H
6NHC
2H
4NH
2Or-C
3H
6NHC
3H
6N (CH
3)
2, consumption is 10% ~ 30% of hydroxy-end capped linear silicone oils, sulfydryl coupling agent and an amino coupling agent gross weight.
Described catalyzer is a Lithium Hydroxide MonoHydrate, and consumption is 50 ~ 500ppm of reactant gross weight.
Three of the object of the invention is: the microemulsion and the application thereof of above-mentioned amino/sulfhydryl co-modified organosilicon polysiloxane are provided.
For realizing above-mentioned purpose, the present invention adopts following technical scheme to realize:
The 1 part of emulsifying agent for preparing is joined in the reactor drum, add 2 parts amino/sulfhydryl co-modified organosilicon polysiloxane again, start stirring; Add phase inversion water earlier; Add the neutralizing acid in early stage, add deionized water while stirring, process solid content and be 30% emulsion; In using at last and about acid for adjusting pH value to 6, obtain the emulsion of zona pellucida blue light.
Described neutralizing acid is: formic acid, Glacial acetic acid min. 99.5 or thionamic acid, consumption are 0.1% ~ 4.0% of the total consumption of microemulsion.
Described microemulsion is applied to the level and smooth finishing composition of textile printing and dyeing, daily-use chemical industry nursing agent.
The main quality index of microemulsion: outward appearance: the liquid that blue light is transparent; Solid content: (1.0 ~ 60) %; Ionic: weak cation; PH value: 6.0 ~ 8.0; Stability: 3000r/min spinning 30min is not stratified, floating oil not.
Advantage of the present invention is: the present invention has made full use of the similar principle that mixes; It is synthetic amino/sulfhydryl co-modified organosilicon polysiloxane of the present invention; Contain in its molecular structure with wool (suede) fibrous molecular structure in identical element sulphur; Thereby when using this soft finishing agent to wool (suede) fabric treating; Wool (suede) fabric to the adsorptive capacity of amino/sulfhydryl co-modified organosilicon polysiloxane much larger than adsorptive capacity, so after utilizing microemulsion that the present invention prepares to wool (suede) fabric treating, the feel of wool (suede) fabric is more plentiful, more smooth, more soft to common amino-modified silicone polysiloxane soft agent.
Embodiment
In order to describe particularly and to explain technical characterstic of the present invention, list following each implementation method, but invention is not limited to following embodiment.
Embodiment 1
(1) amino/build the preparation of basic co-modified organosilicon polysiloxane;
Take into account in the four-hole boiling flask of 1000mL of nitrogen tube in that whisking appliance, prolong, temperature are housed, adding 600g viscosity is the hydroxy-end capped linear silicone oils of 83cs, 22g aminoethyl aminopropyl methyl dimethoxysilane hydrolyzate; 8g mercapto propyl group methyl dimethoxysilane coupling agent stirs and is warming up to 85 ~ 90 ℃, adds Lithium Hydroxide MonoHydrate 0.8g; Behind the stirring reaction 30min; Control reaction temperature is at 105 ~ 110 ℃, and insulation reaction 5h vacuumizes lower-molecular substance.The cooling back leaches solid insoluble with filter screen, gets water white amino/sulfhydryl co-modified organosilicon polysiloxane, and its viscosity is 1200mPa.S, nonvolatile substances content >=99.6% (110 ℃/3h).
(2) 30% preparation of microemulsion:
In the large beaker of 1000mI, add 22g AEO (n=9), 28g AEO (n=5) stirs earlier; Add the 100g amino/sulfhydryl co-modified organosilicon polysiloxane again, stir 10min, add deionized water 20g again; The 2g Glacial acetic acid min. 99.5 after stirring, under agitation slowly adds deionized water 325g; After after water injection continued stirs 30min, add the 3g Glacial acetic acid min. 99.5 at last again and regulate the pH value, obtain at last with the transparent liquid of blue light.
Use:
Above-mentioned 30% microemulsion for preparing is used for the processing to shabri clothing cloth, does blank assay simultaneously.
(1) hand feel finishing technology:
Microemulsion consumption: 35g/L
Dipping (bath raio): 1:10
Bathe temperature: 35 ℃ ~ 40 ℃
Liquid carrying rate: 70% ~ 80%
Drying time/temperature: 4min/100 ℃
Naturally moisture regain: 24 hours.
(2) performance is relatively:
Table 1 performance relatively
As shown in table 1; Fleece fabrics through the amino/sulfhydryl co-modified organosilicon polysiloxane arrangement all has excellent performance on each item index; Have more excellent handle effect than common double ammonia type silicon breast, this just in this finishing composition two kinds of components bring into play synergistic result.
Claims (3)
1. the microemulsion of amino/sulfhydryl co-modified organosilicon polysiloxane is characterized in that:
The 1 part of emulsifying agent for preparing is joined in the reactor; The amino/sulfhydryl co-modified organosilicon polysiloxane that adds 2 parts again; Start stirring; Add phase inversion water earlier; Add the neutralizing acid in early stage, add deionized water while stirring, make solid content and be 30% emulsion; In using at last and about acid for adjusting pH value to 6, obtain the emulsion of oolemma blue light;
Said amino/sulfhydryl co-modified organosilicon polysiloxane, its structural formula is following:
Wherein: A, B, C are positive integer and A>B >=C;
A=0~2500；
B=0~80；
C=0~50；
R is-OH ,-CH
3,-OCH
3
R
1For-C
3H
6NHC
2H
4NH
2Or-C
3H
6NH C
3H
6N (CH
3)
2
R
2For-SC
3H
6Si (OCH
3)
2CH
3Or-SC
3H
6Si (OC
2H
5)
2CH
3
2. the microemulsion of amino/sulfhydryl co-modified organosilicon polysiloxane according to claim 1, it is characterized in that: described neutralizing acid is: formic acid, Glacial acetic acid min. 99.5 or thionamic acid, consumption are 0.1% ~ 4.0% of the total consumption of microemulsion.
3. the microemulsion of amino/sulfhydryl co-modified organosilicon polysiloxane according to claim 1, it is characterized in that: described microemulsion is applied to the level and smooth finishing composition of textile printing and dyeing, daily-use chemical industry nursing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210314241 CN102827377A (en) | 2008-12-09 | 2008-12-09 | Amino/sulfydryl co-modified organosilicon polysiloxane microemulsion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210314241 CN102827377A (en) | 2008-12-09 | 2008-12-09 | Amino/sulfydryl co-modified organosilicon polysiloxane microemulsion |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810177180 Division CN101503514B (en) | 2008-12-09 | 2008-12-09 | Synthesizing method of amino / sulfhydryl co-modified organosilicon polysiloxane |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230797A (en) * | 2021-12-30 | 2022-03-25 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
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2008
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230797A (en) * | 2021-12-30 | 2022-03-25 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
| CN114230797B (en) * | 2021-12-30 | 2023-12-01 | 江苏奥斯佳材料科技股份有限公司 | Cationic organosilicon polymer, microemulsion and preparation method thereof |
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Application publication date: 20121219 |