CN105694062A - Cross-linked structure dendritic amino silicone oil and preparation method thereof - Google Patents
Cross-linked structure dendritic amino silicone oil and preparation method thereof Download PDFInfo
- Publication number
- CN105694062A CN105694062A CN201610083774.4A CN201610083774A CN105694062A CN 105694062 A CN105694062 A CN 105694062A CN 201610083774 A CN201610083774 A CN 201610083774A CN 105694062 A CN105694062 A CN 105694062A
- Authority
- CN
- China
- Prior art keywords
- cross
- linked structure
- silicon oil
- preparation
- amido silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
-
- 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
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- 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
Abstract
The invention discloses cross-linked structure dendritic amino silicone oil.A molecular structure contains chain links shown in Scheme (1), wherein R1, R2 and R3=-CH3--C18H37 or aryl, and R1, R2 and R3 can be identical or different.A preparation method includes: enabling siloxane oligomer and amino silane coupling agent to be in copolymerization reaction at 80-140 DEG C under action of a base catalyst to prepare a linear silicone oil intermediate; adding oligomeric silsesquioxane resin containing trifunctional/tetrafunctional silica chain links in structure for reaction at 130-160 DEG C for 0.5-2 h to obtain a copolymer which is the cross-linked structure dendritic amino silicone oil.The cross-linked structure dendritic amino silicone oil is emulsified into stable silicone latex by using isoalcohol polyoxyethylene ether to be used for softening aftertreatment of fiber fabric, and the fabric can be given more excellent soft, fluffy and loose hand feeling.
Description
Technical field
The invention belongs to textile finshing agent technical field, particularly to a kind of cross-linked structure dendroid amido silicon oil and preparation method thereof。
Background technology
Amino silicone, the i.e. abbreviation of ammonia alkyl polysiloxanes or amido silicon oil。Amino silicone, Final finishing for fabric, the smooth performance of softness and the feel of fabric can not only be improved, and crease-resistant, the antistatic property that fabric is certain can be given, thus become the class function additive that the soft Final finishing field of weaving is most widely used, but how to improve its application performance and feel further, interesting。
There is hyperbranched or crosslinking in the structure making amido silicon oil, the film property of amino silicone can be effectively improved under the suitable condition of mean molecule quantity, improve the soft of amino silicone institute finish fabric, sliding, bullet, very performance and active sense, and can imparting process after fabric with other performances or hands sense, as publication number utilizes end ring oxygen polyether block silicone oil and diethylenetriamine to react synthesized hyperbranched cross-linked structure polyethers amino block organosilicon disclosed in the patent documentation of [CN104650364], can not only cohesive force between fortifying fibre, and the good soft and full property of fabric and washable feel can be given。But, how document synthesizes desired hyperbranched, the resinoid amido silicon oil of cross-linked structure with short-cut method, rarely has report。
Another compared with linear amino-silicone oil, the resinoid amido silicon oil of cross-linked structure, good soft fluffy feel can be shown in low-viscosity situation, the amido silicon oil of kindred circumstances lower linear structure then needs high viscosity to can be only achieved same finishing effect, but, in actual production, high viscosity can increase the roll banding risk in the emulsifying difficulty of amido silicon oil and use procedure。
Polymerisation in bulk is a kind of method that synthesizing amino silicone oil is the most frequently used, this point visible publication number respectively document such as [CN102021838], [CN104233821]。So, in the building-up process of amido silicon oil, can utilizing the amido silicon oil of linear amino-silicone oil next synthesizing cross-linked structure tree smectic with the polycondensation reaction of highly cross-linked oligomeric silsesquioxane resin and so as to produce active feel, there is not been reported。
Summary of the invention
For overcoming above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of highly branched, cross-linked structure resin-like amido silicon oil and preparation method thereof, for the Final finishing of fabric after amido silicon oil emulsifying prepared by this method, performance endured by the smooth bullet of softness that can not only be obviously improved fabric, and can give the active fluffy sense that fabric is comfortable。
For achieving the above object, the technical solution used in the present invention is:
A kind of cross-linked structure dendroid amido silicon oil, containing Scheme(1 in molecular structure) shown in chain link:
In formula, R1、R2、R3=-CH3～-C18H37Or aryl, R1、R2、R3May be the same or different；
The preparation method of described cross-linked structure dendroid amido silicon oil, comprises the following steps:
The first step, weighs siloxane oligomer body and amino silane, stirring and evenly mixing successively by linear silicone oils intermediate ammonia value desired ratio, is denoted as material A, is heated to 80-140o С, add material A quality (1-6) × 10-4The base catalyst of %, first atmospheric agitation 30min, the more de-low 10-15min that boils of decompression when gauge pressure is 500-550mmHg, the continuous copolyreaction 3-6h of temperature control 80-140o С again, obtain transparent thick liquid, namely containing linear silicone oils intermediate ammonia alkyl methylsiloxane-co-dimethylsiloxane copolymer (AAPS) of chain link shown in Scheme (1) (a)-(b) in structure, viscosity is about 100-5000mPa.s, ammonia value is 0.1-0.9mmol/g；
The mass ratio of the copolyreaction of described siloxane oligomer body and amino silane, siloxane oligomer body and amino silane depends on the ammonia value of linear silicone oils intermediate；
Second step, in intermediate reaction system, adds in the oligomeric silsesquioxane resin (having another name called organic siliconresin) of intermediate quality 5-20% structure highly-branched, after stirring and evenly mixing, at N2Temperature control 130-160o С stirring reaction 0.5-2h under protective condition, after be down to 40-45o С, with in acetic acid and base catalyst, being clear to slightly muddy shape liquid or elastomer, i.e. cross-linked structure dendroid amido silicon oil, ammonia value is 0.05-0.88mmol/g。
Described siloxane oligomer body, including octamethylcy-clotetrasiloxane (D4), siloxanes ring body (DMC), structure be HO [(CH3)2SiO]30-33The linear body hydroxy silicon oil of H, viscosity are micromolecular hydroxyl silicone oil and their the arbitrary proportion mixture of 20-100mPa.s。
Described amino silane is two senses containing primary, secondary, tertiary amine alkyl or trifunctional alkoxy silane in molecular structure。
Described amino silane includes N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane (KH-602), N, N-dimethyl-γ-aminopropyl-γ-aminopropyltriethoxy dimethoxysilane (KH-121), piperazinopropyl methyl dimethoxysilane (GP-108), N-cyclohexyl-γ-aminopropyltrimethoxysilane, diethylenetriamine base hydroxypropyl methyl dimethoxy silane (KH-941), γ-aminopropyltriethoxy dimethoxysilane (KH-551), γ-aminopropyltriethoxy diethoxy silane, polyethers amido hydroxypropyl methyl dimethoxysilane, the arbitrary proportion mixture of these silane and the hydrolytie polycondensation thing of these silane。
Described base catalyst is the inorganic or organic alkali of Si-O bond fission in energy catalysis organosiloxane oligomer。
Described base catalyst includes potassium hydroxide, sodium hydroxide, Tetramethylammonium hydroxide·5H2O, tetramethyl hydroxide and by these alkali and D4, prepared silicon alkoxide such as the decamethyl silanol potassium, alkali glue of DMC reaction。
Described oligomeric silsesquioxane resin, for containing (c)-(e) chain link shown in Scheme (1) or containing the organic siliconresin of (a) and (c)-(e) chain link, structure highly-branched simultaneously in molecular structure。
Described oligomeric silsesquioxane resin includes poly methyl silsesquioxane, polyphenylsilsesquioxane, the modified MQ resin of methyl, phenyl modified MQ resin, ethyl or octyl group or the modified MQ resin of cetyl and the modified MQ resin of PolydimethylsiloxaneChain Chain section。
Described cross-linked structure dendroid amido silicon oil, containing the multiple chain link of (a)-(e) shown in Scheme (1) in structure, general transparent shape flowable liquid under degree of cross linking appropraite condition, viscosity is 2000-10000mPa.s, is illiquidity visco-elastic body or elastic solid (Hookean body) when cross-linking transition。
The cross-linked structure dendroid amido silicon oil of the present invention is applied in weaving, step is as follows: namely take cross-linked structure dendroid amido silicon oil (DAPS), ethylene glycol monobutyl ether cosolvent and the 30-50% isomery fatty alcohol-polyoxyethylene ether emulsifying agent of 30-50% is added by silicone oil quality, mechanical agitation mixes, then the deionized water of metering is slowly added while stirring, so as to being diluted to solid content is 15%, obtain translucent-emulsion with blue-fluorescence, be DAPS silicon breast。Then, DAPS silicon breast water is diluted in proportion and is made into work body lotion, then fabric be impregnated in an immersing and rolling in this body lotion, then take out, fabric is dried at 100o С, shapes 90s at 160o С again, can the bullet property endured and the active feel of soft comfortable。
Except for textile finishing, the cross-linked structure dendroid amido silicon oil of the present invention, moreover it can be used to personal care and toiletry, the preparation of daily use chemicals softener and the aspect such as yarn, eider down soft treatment。
Beneficial effects of the present invention: the present invention utilizes siloxane oligomer body and amino silane first to carry out bulk copolymerization and linear structure amido silicon oil intermediate ammonia alkyl methylsiloxane-co-dimethylsiloxane copolymer AAPS is synthesized, then again the oligomeric silsesquioxane resin of AAPS Yu structure height branching is carried out high-temperature polycondensation balancing response, start a new method preparing highly-branched, cross-linked structure dendroid amido silicon oil, and amino silicone prepared by this method is for textile finishing, can also give the active feel that fabric is comfortable while improving the smooth performance of fabric sofetening。
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the present invention is not restricted to these embodiments。
A kind of cross-linked structure dendroid amido silicon oil, containing Scheme(1 in molecular structure) shown in chain link:
In formula, R1、R2、R3=-CH3～-C18H37Or aryl, R1、R2、R3May be the same or different；
Embodiment 1
Have in the three-necked bottle of thermometer, reflux condensing tube and motor stirrer at device, be sequentially added into 100gD in proportion4, 1.1gN-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, stirring and evenly mixing, be denoted as material A；Material A is heated to 80o С, adds 2.02 × 10-4G potassium hydroxide is (in material A quality 2 × 10-4%) catalyst, first atmospheric agitation 30min, the de-low 10min that boils of decompression when gauge pressure is 500-550mmHg again, then temperature control 85o С continuous stirring reaction 6h, obtain transparent thick liquid, namely containing R in chain link, formula shown in Scheme (1) (a)-(b) in structure1=R2=-CH3、A=-NHC2H4NH2, total amount is about the linear silicone oils intermediate N β-aminoethyl-γ-aminopropyltriethoxy siloxanes-co-dimethylsiloxane copolymer of 100.8g, is denoted as AAPS-1, and viscosity is 4910mPa.s, ammonia value is 0.1mmol/g；
In above-mentioned intermediate A APS-1 reaction system, adding the oligomeric methyl silsesquioxane MQ resin of (in AAPS mass 5%) 5.0g, stirring and evenly mixing, at N2It is stirred under protective condition being heated to 160o С insulation reaction 2h; then, it is down to 40o С, with in acetic acid and base catalyst; obtain transparence flowable liquid, namely containing R in chain link, formula shown in Scheme (1) (a)-(e) in structure1=R2=-CH3、R2=-CH3、A=-NHC2H4The cross-linked structure dendroid amido silicon oil of NH, ammonia value is 0.095mmol/g, and viscosity is 6300mPa.s。
Embodiment 2
Have in the three-necked bottle of thermometer, reflux condensing tube and motor stirrer at device, be sequentially added into 60gD in proportion4, Wacker company of 30gDMC, 10g linear body hydroxy silicon oil 62M(Germany), 12.29gN, N-dimethyl-γ-aminopropyl-γ-aminopropyltriethoxy dimethoxysilane (KH-121) stirring and evenly mixing, be denoted as material A；Material A is heated to 100o С, then, adds containing 2.2 × 10-4The decamethyl silanol potassium catalyst of g potassium hydroxide (in material A 2 × 10-4%), first atmospheric agitation 30min, the de-low 15min that boils of decompression when gauge pressure is 550mmHg again, then temperature control 100o С continuous stirring reaction 4h, obtain transparent thick liquid, namely containing chain link shown in Scheme (1) (a)-(b) in structure, R1=R2=-CH3 in formula, A=-NHC3H6N (CH3) 2, total amount is about the linear silicone oils intermediate N of 110.0g, N-dimethyl-γ-aminopropyl-γ-aminopropyltriethoxy siloxanes-co-dimethylsiloxane copolymer, it is denoted as AAPS-2, viscosity is about 280mPa.s, ammonia value is 0.88mmol/g。
In above-mentioned intermediate A APS-2 reaction system, add AAPS mass 20% that is about 22.0g structure contain R in Scheme (1) (c), Scheme (1) (d), Scheme (1) (e) shown three kinds of chain links, formulas3=-C16H33The modified oligomeric silsesquioxane of Long carbon chain cetyl (having another name called the modified MQ resin of cetyl) stirring and evenly mixing, at N2It is stirred under protective condition being heated to 130o С insulation reaction 0.5h; then, it is down to 45o С, with in acetic acid and base catalyst; obtain transparence flowable liquid, namely containing R in Scheme (1) (a)-(e) shown five kinds of chain links, formulas in structure1=R2=-CH3、R3=-C16H33、A=NHC3H6N(CH3)2Cross-linked structure dendroid amido silicon oil, ammonia value is 0.73mmol/g, and viscosity is 2080mPa.s。
Embodiment 3
Have in the three-necked bottle of thermometer, reflux condensing tube and motor stirrer at device, it is sequentially added into hydroxyl endblocked polydimethylsiloxane (Tangshan three friend's silicon industry Limited Liability), 7.7g γ-gamma-piperazinepropyl methyldimethoxysilane (GP-108) stirring and evenly mixing that 60.0g siloxanes ring body DMC, 40.0g viscosity is 60mPa.s in proportion, is denoted as material A；Material A is heated to 120o С, then, adds 4.0 × 10-4G Tetramethylammonium hydroxide is (in material A 3.7 × 10-4%) catalyst, first atmospheric agitation 30min, then when gauge pressure is 500mmHg, decompression takes off the low 10min that boils, then temperature control 120o С continuous stirring reaction 5h, obtain transparent thick liquid, namely containing R in chain link, formula shown in Scheme (1) (a)-(b) in structure1=R2=-CH3, A=piperazinyl, total amount is about the linear silicone oils intermediate γ-piperazinyl-propyl methylsiloxane-co-dimethylsiloxane copolymer of 106.0g, is denoted as AAPS-3, and viscosity is 900mPa.s, ammonia value is 0.6mmol/g；
In above-mentioned intermediate A APS-3 reaction system, add AAPS mass 9.4% that is 10.0g structure contain R in chain link, formula shown in Scheme (1) (c)-(e)3=-C6H5Phenyl modified poly methyl silsesquioxane resin agitating mixing, at N2It is stirred under protective condition being heated to 145o С insulation reaction 1h; then, it is down to 43o С, with in acetic acid and base catalyst; obtain transparence flowable liquid, namely containing the shown five kinds of chain links of Scheme (1) (a)-(e), A=piperazine, R in structure1=R2=-CH3、R3=-C6H5Cross-linked structure dendroid amido silicon oil, ammonia value is 0.57mmol/g, and viscosity is 3230mPa.s。
Embodiment 4
Have in the three-necked bottle of thermometer, reflux condensing tube and motor stirrer at device, be sequentially added into 100g linear body 9701(Japan XINYUE in proportion), 3.4gN-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane (KH-602) stirring and evenly mixing, be denoted as material A；Material A is heated to 105o С, then adds containing 1.6 × 10-4G potassium hydroxide is (in material A 1.55 × 10-4Alkali glue catalyst %), first atmospheric agitation 30min, the de-low 12min that boils of decompression when gauge pressure is 530mmHg again, then temperature control 105o С continuous stirring reaction 4.5h, obtain transparent thick liquid, namely containing chain link shown in Scheme (1) (a)-(b), R in formula in structure1=R2=-CH3、A=-NHC2H4NH2, total amount is the linear amino-silicone oil intermediate N β-aminoethyl-γ-aminopropyltriethoxy siloxanes-co-dimethylsiloxane copolymer of 103.0g, is denoted as AAPS-4, and viscosity is 3600cPa.s, ammonia value is 0.3mmol/g。
In above-mentioned intermediate A APS-4 reaction system, add AAPS mass 6.5% that is 6.63g structure contain R in Scheme (1) (a), Scheme (1) (c), Scheme (1) (e) shown three kinds of chain links, formulas1=R2=R3=-CH3The polydimethylsiloxane--modified oligomeric methyl silsesquioxane resins of structure highly-branched, stirring and evenly mixing, at N2It is stirred under protective condition being heated to 140o С insulation reaction 1h; then; it is down to 45o С; with in acetic acid and base catalyst; obtain transparence flowable liquid, namely containing R in Scheme (1) (a)-(c), Scheme (1) (e) shown four kinds of chain links, formulas in structure1=R2=R3=-CH3、A=-NHC2H4NH2Cross-linked structure dendroid amido silicon oil, ammonia value is 0.3mmol/g, and viscosity is 5800mPa.s。
Cross-linked structure dendroid amido silicon oil 20g prepared by Example 1-4, add 40% that is the ethylene glycol monobutyl ether cosolvent of 8g and 50% that is 10g isomerous tridecanol polyoxyethylene ether 1330/1390 emulsifying agent, mechanical agitation mixes, pH=6 is adjusted with acetic acid, add 162g deionized water while stirring, make the emulsion that solid content is 15%；Then, take the emulsion that 2g solid content is 15%, be made into arrangement work body lotion with the dilution of 100g water；Taking area again is 16.3cm × 12.6cm(warp × latitude) the textile embryo cloth (specification 21 × 21 × 108 × 98) of white, it is impregnated in work body lotion with laboratory room small-sized padding machine one immersing and rolling, pick-up about 70%；By fabric 100 DEG C dry 5min, at 160 DEG C of baked and cured 90s, then at equilibrium at room temperature 24h, carry out performance test；The bullet property endured represents with creasy recovery angle, is measured with the intellectual fabric crease elasticity test instrument of YG (B) 541E, and soft and active feel digital palpation for examination of trauma is evaluated。
In another Example 1-4, uncrosslinked modified linear amino silicone is used as the reference of the present invention, and the application performance measurement result of the bafta arranged is in Table 1。
。
Claims (10)
1. the preparation method of a cross-linked structure dendroid amido silicon oil, it is characterised in that containing Scheme(1 in molecular structure) shown in chain link:
In formula, R1、R2、R3=-CH3～-C18H37Or aryl, R1、R2、R3May be the same or different；
。
2. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 1, it is characterised in that comprise the following steps:
The first step, weighs siloxane oligomer body and amino silane, stirring and evenly mixing successively by linear silicone oils intermediate ammonia value desired ratio, is denoted as material A；Material A is heated to 80-140o С, adds material A quality (1-6) × 10-4The base catalyst of %, first atmospheric agitation 30min, the more de-low 10-15min that boils of decompression when gauge pressure is 500-550mmHg, the continuous copolyreaction 3-6h of temperature control 80-140o С again, obtain transparent thick liquid, i.e. linear silicone oils intermediate ammonia alkyl methylsiloxane-co-dimethylsiloxane copolymer (AAPS) containing chain link shown in Scheme (1) (a)-(b) in structure, viscosity is 100-5000mPa.s, ammonia value is 0.1-0.9mmol/g；
The mass ratio of the copolyreaction of described siloxane oligomer body and amino silane, siloxane oligomer body and amino silane is the ammonia value depending on linear silicone oils intermediate；
Second step, in intermediate reaction system, adds in the oligomeric silsesquioxane resin of intermediate quality 5-20% structure highly-branched, after stirring and evenly mixing, at N2Temperature control 130-160o С stirring reaction 0.5-2h under protective condition, after be down to 40-45o С, with in acetic acid and base catalyst, being clear to slightly muddy shape liquid or elastomer, i.e. cross-linked structure dendroid amido silicon oil, ammonia value is 0.05-0.88mmol/g。
3. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 2, it is characterised in that described siloxane oligomer body, including octamethylcy-clotetrasiloxane (D4), siloxanes ring body (DMC), structure be HO [(CH3)2SiO]30-33The linear body hydroxy silicon oil of H, viscosity are micromolecular hydroxyl silicone oil and their the arbitrary proportion mixture of 20-100mPa.s。
4. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 2, it is characterised in that described amino silane is two senses containing primary, secondary, tertiary amine alkyl or trifunctional alkoxy silane in molecular structure。
5. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 4, it is characterized in that, described amino silane includes N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane (KH-602), N, N-dimethyl-γ-aminopropyl-γ-aminopropyltriethoxy dimethoxysilane (KH-121), piperazinopropyl methyl dimethoxysilane (GP-108), N-cyclohexyl-γ-aminopropyltrimethoxysilane, diethylenetriamine base hydroxypropyl methyl dimethoxy silane (KH-941), γ-aminopropyltriethoxy dimethoxysilane (KH-551), γ-aminopropyltriethoxy diethoxy silane, polyethers amido hydroxypropyl methyl dimethoxysilane, the arbitrary proportion mixture of these silane and the hydrolytie polycondensation thing of these silane。
6. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 2, it is characterised in that described base catalyst is can the inorganic or organic alkali of Si-O bond fission in catalysis organosiloxane oligomer。
7. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 6, it is characterised in that described base catalyst includes potassium hydroxide, sodium hydroxide, Tetramethylammonium hydroxide·5H2O, tetramethyl hydroxide and by these alkali and D4, prepared silicon alkoxide such as the decamethyl silanol potassium, alkali glue of DMC reaction。
8. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 2, it is characterized in that, described oligomeric silsesquioxane resin, for containing (c)-(e) chain link shown in Scheme (1) or containing the oligomeric silsesquioxane of Scheme (1) (a) and (c)-(e) chain link, structure highly-branched simultaneously in molecular structure。
9. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 8, it is characterized in that, described oligomeric silsesquioxane resin includes poly methyl silsesquioxane, polyphenylsilsesquioxane, the modified MQ resin of methyl, phenyl modified MQ resin, ethyl or octyl group or the modified MQ resin of cetyl and the modified MQ resin of PolydimethylsiloxaneChain Chain section。
10. the preparation method of a kind of cross-linked structure dendroid amido silicon oil according to claim 2, it is characterized in that, described cross-linked structure dendroid amido silicon oil, containing the multiple chain link of (a)-(e) shown in Scheme (1) in structure, general transparent shape flowable liquid under degree of cross linking appropraite condition, viscosity is 2000-10000mPa.s, is illiquidity visco-elastic body or elastic solid (Hookean body) when cross-linking transition。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610083774.4A CN105694062A (en) | 2016-02-06 | 2016-02-06 | Cross-linked structure dendritic amino silicone oil and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610083774.4A CN105694062A (en) | 2016-02-06 | 2016-02-06 | Cross-linked structure dendritic amino silicone oil and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105694062A true CN105694062A (en) | 2016-06-22 |
Family
ID=56222138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610083774.4A Pending CN105694062A (en) | 2016-02-06 | 2016-02-06 | Cross-linked structure dendritic amino silicone oil and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105694062A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750185A (en) * | 2017-03-06 | 2017-05-31 | 山东清硕环境科技有限公司 | A kind of Amino End Group Carbonsilane dendrimer curing agent and the chimney anticorrosion special-purpose nanometer hybridized polymer prepared based on the curing agent |
| CN107129578A (en) * | 2017-06-21 | 2017-09-05 | 唐山三友硅业有限责任公司 | The preparation method of network structure amino-modified silicone oil finishing agent |
| CN108442119A (en) * | 2018-02-10 | 2018-08-24 | 汪逸凡 | A kind of mercerized wool fluent movement agent and preparation method thereof |
| CN113024816A (en) * | 2021-03-30 | 2021-06-25 | 中国日用化学研究院有限公司 | Comb-type aminosiloxane-allyl polydimethylsiloxane co-modified organic silicon and preparation method thereof |
| CN114957670A (en) * | 2022-06-23 | 2022-08-30 | 佛山市顺德区德美瓦克有机硅有限公司 | Highly-branched cross-linked polysiloxane and waterproof agent |
| CN115093569A (en) * | 2022-01-24 | 2022-09-23 | 广东轻工职业技术学院 | Modified amino silicone oil, preparation method and application thereof in preparation of protein repair hair conditioner |
| CN115505271A (en) * | 2022-09-20 | 2022-12-23 | 杭州赛肯新材料技术有限公司 | Daily chemical personal care organosilicon emulsion and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675652A (en) * | 2012-05-18 | 2012-09-19 | 陕西科技大学 | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil |
| CN102911367A (en) * | 2012-11-12 | 2013-02-06 | 浙江汉邦化工有限公司 | Preparation method of cross-linked block amino-modified silicone oil |
| CN103255618A (en) * | 2012-10-29 | 2013-08-21 | 苏州大学 | Terylene fabric deepening agent copolymer emulsion and preparation method thereof |
| CN103819680A (en) * | 2014-02-25 | 2014-05-28 | 宁波润禾化学工业有限公司 | Preparation method for amino modified silicone oil through sealing end of methoxyl |
| CN103937001A (en) * | 2014-03-28 | 2014-07-23 | 陕西科技大学 | Method for preparing water-dispersible alkyl/polyether amino-silicon resin |
| CN104650364A (en) * | 2015-02-05 | 2015-05-27 | 南通斯恩特纺织科技有限公司 | Preparation method of hyper-branched polyether amide block silicone |
-
2016
- 2016-02-06 CN CN201610083774.4A patent/CN105694062A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675652A (en) * | 2012-05-18 | 2012-09-19 | 陕西科技大学 | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil |
| CN103255618A (en) * | 2012-10-29 | 2013-08-21 | 苏州大学 | Terylene fabric deepening agent copolymer emulsion and preparation method thereof |
| CN102911367A (en) * | 2012-11-12 | 2013-02-06 | 浙江汉邦化工有限公司 | Preparation method of cross-linked block amino-modified silicone oil |
| CN103819680A (en) * | 2014-02-25 | 2014-05-28 | 宁波润禾化学工业有限公司 | Preparation method for amino modified silicone oil through sealing end of methoxyl |
| CN103937001A (en) * | 2014-03-28 | 2014-07-23 | 陕西科技大学 | Method for preparing water-dispersible alkyl/polyether amino-silicon resin |
| CN104650364A (en) * | 2015-02-05 | 2015-05-27 | 南通斯恩特纺织科技有限公司 | Preparation method of hyper-branched polyether amide block silicone |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750185A (en) * | 2017-03-06 | 2017-05-31 | 山东清硕环境科技有限公司 | A kind of Amino End Group Carbonsilane dendrimer curing agent and the chimney anticorrosion special-purpose nanometer hybridized polymer prepared based on the curing agent |
| CN107129578A (en) * | 2017-06-21 | 2017-09-05 | 唐山三友硅业有限责任公司 | The preparation method of network structure amino-modified silicone oil finishing agent |
| CN108442119A (en) * | 2018-02-10 | 2018-08-24 | 汪逸凡 | A kind of mercerized wool fluent movement agent and preparation method thereof |
| CN113024816A (en) * | 2021-03-30 | 2021-06-25 | 中国日用化学研究院有限公司 | Comb-type aminosiloxane-allyl polydimethylsiloxane co-modified organic silicon and preparation method thereof |
| CN115093569A (en) * | 2022-01-24 | 2022-09-23 | 广东轻工职业技术学院 | Modified amino silicone oil, preparation method and application thereof in preparation of protein repair hair conditioner |
| CN114957670A (en) * | 2022-06-23 | 2022-08-30 | 佛山市顺德区德美瓦克有机硅有限公司 | Highly-branched cross-linked polysiloxane and waterproof agent |
| CN115505271A (en) * | 2022-09-20 | 2022-12-23 | 杭州赛肯新材料技术有限公司 | Daily chemical personal care organosilicon emulsion and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105694062A (en) | Cross-linked structure dendritic amino silicone oil and preparation method thereof | |
| CN102675652B (en) | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil | |
| AU608977B2 (en) | Treatment of fibrous materials | |
| AU624263B2 (en) | Stable emulsions containing amino polysiloxanes and silanes for treating fibers and fabrics | |
| CN103214676B (en) | A kind of terpolymer block silicone oil synthetic method | |
| TW538096B (en) | Nitrogen atom-containing polysiloxanes, their preparation, and fiber and fabric finishing agent compositions | |
| JP2821037B2 (en) | Processing method of fiber material | |
| CN103351469B (en) | A kind of preparation method of block silicone oil softening agent | |
| CN105694046A (en) | Preparation method of highly-branched block polyether-aminosiloxane finishing agent | |
| CN104650364B (en) | A kind of preparation method of hyperbranched polyether amino block organosilicon | |
| US5025076A (en) | Silicone-based fabric finishing agent | |
| CN102021838B (en) | Low-yellowing organic silicon softener, preparation method and application thereof | |
| CN101367942B (en) | Preparation method for branched chain type amino-long chain alkyl co-modified silicone oil and its microemulsion, and uses thereof | |
| CN107129578A (en) | The preparation method of network structure amino-modified silicone oil finishing agent | |
| JPH0243224A (en) | Organosilicone compound | |
| CN101805994A (en) | Organosilicon emulsion used for hand feel finishing of wool and blended yarn thereof and preparation method and application thereof | |
| CN101003947A (en) | Finishing agent of polysiloxane fiber, and producing method | |
| CN102952273A (en) | Amphion type amino silicone oil and preparation method thereof | |
| JP2846058B2 (en) | Processing method of fiber material | |
| CN109824900A (en) | Deep silicone oil of the amino modified increasing of one kind and preparation method thereof | |
| CN111019139B (en) | Preparation method of self-emulsifying block copolymerized silicone oil emulsion | |
| CN106835713A (en) | A kind of organosilicon high-elastic smooth finishing agent and preparation method thereof | |
| CN103113590A (en) | Quaternary ammonium base organopolysiloxane high-molecular compound and preparation method and application thereof | |
| JP2008121182A (en) | Method for treatment of fiberfill fibers with aqueous dispersion of organopolysiloxane | |
| JP2865489B2 (en) | Organosilicon compounds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160622 |