CN102517900A - Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane - Google Patents
Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane Download PDFInfo
- Publication number
- CN102517900A CN102517900A CN2011102973863A CN201110297386A CN102517900A CN 102517900 A CN102517900 A CN 102517900A CN 2011102973863 A CN2011102973863 A CN 2011102973863A CN 201110297386 A CN201110297386 A CN 201110297386A CN 102517900 A CN102517900 A CN 102517900A
- Authority
- CN
- China
- Prior art keywords
- special
- weight portions
- preparation
- catalyst
- finishing agent
- 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
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention discloses a finishing agent capable of endowing thick and smooth feel style and a preparation method of special polysiloxane. A market sale routine finishing agent using polyurethane resin performed polymer solution as a main material is added with 2-10 wt% of special polysiloxane to form the finishing agent capable of endowing thick and smooth feel style. The preparation method of the special polysiloxane comprises steps of: adding unreacted solvent and reactant according to a proportion into a reaction container with heating, cooling and backflow condensation apparatuses; adding catalyst with a stirring round of 60-500 r/ min; stirring and heating to 80-150 DEG C and carrying out a backflow reaction for 3-8 h; stirring and cooling to a room temperature; and examining and discharging to obtain the special polysiloxane. The finishing agent added with the special polysiloxane of the invention not only endows thick, plump, fine and smooth hand feel style on polyurethane artificial leather, but also has advantages of long-lasting style after finishing and stable storage of the finishing agent.
Description
Technical field
The present invention relates to the polyurethane artificial leather finishing agent, be specifically related to a kind of finishing agent of thick sliding sense style and preparation method of special polysiloxanes of giving, belong to field of new.
Background of invention
The polyurethane artificial leather finishing agent plays key effect to the functionalization and the application direction of polyurethane artificial leather, and abundant full, fine and smooth, the smooth style of feel has the vast market space in the Application Areas of clothing leather, sofa artificial leather and upper leather.For reaching this style, be employed in generally in the existing finishing agent production technology that quantitative conventional dimethyl silicone polymer or the silicon rubber of interpolation reaches this purpose in the polyurethane resin prepolymer solution.Proved that the polyurethane artificial leather finishing agent that has added conventional dimethyl silicone polymer (the for example dimethicone of viscosity 350 ~ 10000mpa.s) can give the artificial leather smooth hand feeling; But there are not thick sense or thick sense obviously not enough, even it is also of no avail to increase tret; The polyurethane artificial leather finishing agent that has added conventional silicon rubber (the for example one-component of the methyl vinyl silicone rubber of mean molecule quantity 50 ~ 600,000 or platinum group catalyst or dual composition addition type liquid silastic) can reach abundant full, fine and smooth, smooth style, but exists style to keep lasting or finishing agent to deposit the shortcoming of instability (silicon rubber be added on being separated appears in the process of depositing in the finish solution or liberation of hydrogen flatulence causes being difficult to satisfy Practical Performance).
Summary of the invention
The objective of the invention is to overcome the deficiency that existing finishing agent exists; Provide and give thick sliding the feel finishing agent of style and the preparation method of special polysiloxanes; The finishing agent that adds special polysiloxanes preparation not only can make polyurethane artificial leather produce abundant full, fine and smooth, the smooth style of feel, and the style that has after the covering with paint keeps advantage lasting, the finishing agent stable storage.
The finishing agent of giving thick sliding sense style of the present invention comprises following composition: the solid content of 40 ~ 60% weight portions is 30 ~ 40% polyurethane resin prepolymer solution; The special polysiloxanes of 2 ~ 10% weight portions, the white carbon delustering agent of 0 ~ 10% weight portion, the polyether modified siloxane levelling agent of 1 ~ 3% weight portion; The DMF of 10 ~ 20% weight portions; The ethyl acetate of 10 ~ 20% weight portions, the toluene of 10 ~ 20% weight portions adds up to each component 100%;
Wherein said special polysiloxanes has following molecular formula:
Special polysiloxanes shown in the above-mentioned molecular formula is a kind of big molecule modified polyorganosiloxane that on the polysiloxanes side chain, contains long-chain dimethyl silicone polymer and aryl simultaneously or contain long-chain dimethyl silicone polymer, aryl and alkyl simultaneously; Described polyurethane resin prepolymer solution; Be meant the polyurethane resin prepolymer solution of the solid content 30 ~ 40% that forms by isocyanates and PPG or PEPA reaction that does not contain said special polysiloxanes; Be furnished with DMF, toluene, ethyl acetate, acetone or the butanols solvent of 60 ~ 70% weight portions in the solution, such polyurethane resin prepolymer solution is easy to buy from market; Described white carbon delustering agent is meant specific area 250 ~ 350m
2The precipitation method of/g or vapor phase method delustring white carbon, typical supplier and commodity have the K500 of Degussa, the N20 of watt gram, and delustering agent is easy to buy from market; Described polyether modified siloxane is meant that siloxane chain has the silicone surfactant of APEO or polyethenoxy ether or oxygen ethylene oxy propylene random copolymerization polyethers, represents commodity that DC-193 is arranged, and silicone surfactant is easy to buy from market.
Wherein, when being cloudy surface after covering with paint, lacquer, colour wash, etc., add the white carbon delustering agent of 4 ~ 10% weight portions; When being bright after covering with paint, lacquer, colour wash, etc., do not add the white carbon delustering agent.
Wherein, the preparation method of special polysiloxanes comprises following two steps in order:
One, has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A of a trimethyl silicon based end-blocking simultaneously: the vinyl pentamethyl disiloxane that in agitated reactor, adds 1 ~ 10% weight portion; The dimethyl siloxane ring body of 90 ~ 99% weight portions; 0.02 the TMAH catalyst of ~ 0.05% weight portion; Start and stir 60 ~ 500r/min, be warming up to 80 ~ 110 ℃ of reaction 2～4h, be warming up to 160～180 ℃ then; Destroy catalyst and vacuum 10～30Kpa and pull out low-boiling-point substance 1～3h, get intermediate A; Wherein, the dimethyl siloxane ring body is commodity D
3, D
4, choosing any one kind of them among the DMC; Wherein, the molecular formula of intermediate A is following:
Two, the preparation of special polysiloxanes: contain the not reactive solvents of 30 ~ 80% weight portions and the reactant of 20 ~ 70% weight portions in the preparation raw material of this special polysiloxanes; Reactive solvents is not choosing any one kind of them in the aromatic hydrocarbons, alkane, ethers, ketone, alcohols, ester class between 80 ~ 250 ℃ of the boiling points, and the reactant of 20 ~ 70% weight portions comprises following material: the vinylsiloxane intermediate A; The hydrogen containing siloxane B of hydrogen content 0.5 ~ 1.6%; The reactant C of styrene or a-methyl styrene; Molecular formula is CH
2=CH-(CH
2)
N-2The reactant D that constitutes of a-alkene (n is a positive integer, and n=8 ~ 20); The catalyst E that chooses any one kind of them in Karstedt catalyst or the speier catalyst and constitute; Wherein, the Karstedt catalyst is the platinum complex of divinyl tetramethyl disiloxane; Wherein, the speier catalyst is the aqueous isopropanol of chloroplatinic acid; Wherein, the hydrogen molal quantity of supposing the hydrogen containing siloxane B in the above-mentioned reactant of 20 ~ 70% weight portions is M
B, the molal quantity of intermediate A is M
A, the molal quantity of reactant C is M
C, the molal quantity of reactant D is M
D, M then
B: M
A: M
C: M
D=100:10 ~ 90:10 ~ 90:0 ~ 90, and (M
A+ M
C+ M
D): M
B=1 ~ 1.2:1, catalyst E account for 3 ~ 10ppm of A, B, C, D gross weight in platinum; Wherein, the molecular formula of hydrogen containing siloxane B is following:
Wherein, The preparation process of special polysiloxanes is: have heating and cooling and taking back in the reaction vessel of stream condensing unit; Add not reactive solvents and reactant A, B, C, D respectively by said ratio, stir the catalyst E that revolution 60 ~ 500r/min adds aforementioned proportion down, and stir and be warming up to 80 ~ 150 ℃ of back flow reaction 3 ~ 8h; Stir cooling then and reduce to room temperature, the check blowing gets special polysiloxane solution.
Wherein, the molecular weight of intermediate A is 1500 ~ 20000, degree of polymerization m=20 ~ 250.
The present invention has the following advantages: 1, contain R in the special polysiloxane molecule
2Functional group perhaps removes and contains R
2Functional group can be simultaneously but must not contain R
3Functional group; Increased special polysiloxanes in the resin of commercially available conventional finishing agent and the compatibility in the solvent; Special polysiloxane molecule internal cause like this contains aryl or aralkyl can make the finishing agent stable storage of the present invention that contains this special polysiloxanes; And in 12 months phenomenon of phase separation can not appear, satisfied practical requirement; 2, the numerical values recited of the molecular weight size of described intermediate A or degree of polymerization m plays a crucial role for the thick sense of finishing agent, and the molecular weight of A numerical value more little or degree of polymerization m is more little, and thick sense is not obvious more; Otherwise; Thick sense is obvious more, but the excessive system viscosity that in addition reaction, can cause of the molecular weight of A numerical value excessive or degree of polymerization m is excessive, is unfavorable for stirring; Take all factors into consideration each factor, be advisable (degree of polymerization m=20 ~ 250) between the molecule of intermediate A of the present invention measured 1500 ~ 20000; 3, special polysiloxane molecule of the present invention can be likened into be uniform-distribution with all long long tooth and the assorted comb of short between cog on the handle visually, and the comb handle is equivalent to reactant B, and all long long tooth is equivalent to intermediate A, and the weak point tooth is equivalent to reactant C or C+D; Such molecule is equivalent to become a molecule micelle to many linear molecule ligation of differing in size, and has produced the third dimension in space, and then has caused thick sense effect.
The specific embodiment
Below be preparation embodiment of the present invention, these embodiment only are used to the present invention is described and unrestricted technical scheme of the present invention.
Embodiment 1:
Has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A 1 of a trimethyl silicon based end-blocking simultaneously: add 10g vinyl pentamethyl disiloxane, 990g hexamethyl cyclotrisiloxane (D in the four-hole boiling flask of electronic stirring and heating jacket at 1000ml
3), 0.2g TMAH catalyst, start electronic stirring (60 ~ 500r/min), be warming up to 80 ~ 110 ℃ of reaction 2h, be warming up to then 160 ℃ destroy catalyst and vacuum (10～30Kpa) pull out low-boiling-point substance 2h, molecular formula do
CH
2=CH
2-Si(CH
3)
2O-[(CH
3)
2SiO]
225~235-Si(CH
3)
3
Intermediate A 1 (mean molecule quantity 17000), yield 90%.
Embodiment 2:
Has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A 2 of a trimethyl silicon based end-blocking simultaneously: add 20g vinyl pentamethyl disiloxane, 980g octamethylcy-clotetrasiloxane (D in the four-hole boiling flask of electronic stirring and heating jacket at 1000ml
4), 0.3g TMAH catalyst, start electronic stirring (60 ~ 500r/min), be warming up to 80 ~ 110 ℃ of reaction 3h, be warming up to then 180 ℃ destroy catalyst and vacuum (10～30Kpa) pull out low-boiling-point substance 1h, molecular formula do
CH
2=CH
2-Si(CH
3)
2O-[(CH
3)
2SiO]
110~120-Si(CH
3)
3
Intermediate A 2 (mean molecule quantity 8700), yield 86%.
Embodiment 3:
Has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A 3 of a trimethyl silicon based end-blocking simultaneously: add 50g vinyl pentamethyl disiloxane in the four-hole boiling flask of electronic stirring and heating jacket at 1000ml; 950g commodity DMC (ring siloxane mixture); 0.5g TMAH catalyst; Start electronic stirring (60 ~ 500r/min); Be warming up to 80 ~ 110 ℃ of reaction 4h, (10～30Kpa) pull out low-boiling-point substance 3h, get molecular formula to do to be warming up to 170 ℃ of destruction catalyst and vacuum then
CH
2=CH
2-Si(CH
3)
2O-[(CH
3)
2SiO]
40~50-Si(CH
3)
3
Intermediate A 3 (mean molecule quantity 3500), yield 86%.
Embodiment 4:
Has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A 4 of a trimethyl silicon based end-blocking simultaneously: add 100g vinyl pentamethyl disiloxane, 900g octamethylcy-clotetrasiloxane (D in the four-hole boiling flask of electronic stirring and heating jacket at 1000ml
4), 0.4g TMAH catalyst, start electronic stirring (60 ~ 500r/min), be warming up to 80 ~ 110 ℃ of reaction 3.5h, be warming up to then 160 ℃ destroy catalyst and vacuum (10～30Kpa) pull out low-boiling-point substance 2.5h, molecular formula do
CH
2=CH
2-Si(CH
3)
2O-[(CH
3)
2SiO]
20~25-Si(CH
3)
3
Intermediate A 4 (mean molecule quantity 1700), yield 85%.
Embodiment 5:
Have heating and cooling and take back in the four-hole boiling flask of stream condensing unit at 1000ml, add 500g toluene, 20g hydrogen content 0.5% molecular formula is (CH
3)
3SiO-[(CH
3) (H) Si O]
30[(CH
3)
2SiO]
54-Si (CH
3)
3Reactant B (hydrogen molal quantity 0.1mol); The intermediate A 1 (0.02mol) of 340g embodiment 1; The a-methyl styrene reactant C (0.085mol) of 10g, stir (the Karstedt catalyst E of 60 ~ 500r/min) times adding systems of revolution gross weight 3ppm (in platinum), heating and stirring are warming up to 80 ~ 100 ℃ of back flow reaction 3h; Stir cooling then and reduce to room temperature, the check blowing must contain the toluene solution (representing with G1) of 42% weight portion of special polysiloxanes.
Embodiment 6:
Have heating and cooling and take back in the four-hole boiling flask of stream condensing unit at 1000ml, add the 500g tasteless kerosene, 10g hydrogen content 1.5% molecular formula is (CH
3)
3SiO-[(CH
3) (H) Si O]
24.3Si (CH
3)
3Reactant B (hydrogen molal quantity 0.15mol), the intermediate A 2 (0.05mol) of 435g embodiment 2, the styrene reactant C (0.06mol) of 6g, the CH of 8g
2=CHC
12H
25Reactant D (0.04mol); (revolution adds the speier catalyst E that accounts for system gross weight 4ppm (in platinum) 60 ~ 500r/min) times in stirring; Heating and stirring are warming up to 120 ~ 140 ℃ of back flow reaction 4h; Stir cooling then and reduce to room temperature, the check blowing must contain the kerosin (representing with G2) of 48% weight portion of special polysiloxanes.
Embodiment 7:
Have heating and cooling and take back in the four-hole boiling flask of stream condensing unit at 1000ml, add the detergent alkylate of 300g, 50g hydrogen content 0.8% molecular formula is:
(CH
3)
3SiO-[(CH
3)(H)Si?O]
46[(CH
3)(C
6H
5)Si?O]?
10[(CH
3)
2Si?O]
20-Si(CH
3)
3
Reactant B (hydrogen molal quantity 0.4mol), the intermediate A 4 (0.2mol) of 340g embodiment 4, the CH of 23g
2=CHC
6H
13Reactant D (0.2mol); (revolution adds the speier catalyst E that accounts for system gross weight 5ppm (in platinum) 60 ~ 500r/min) times in stirring; Heating and stirring are warming up to 100 ~ 120 ℃ of back flow reaction 6h; Stir cooling then and reduce to room temperature, the check blowing must contain the alkylbenzene solution (representing with G3) of 60% weight portion of special polysiloxanes.
Embodiment 8:
Have heating and cooling and take back in the four-hole boiling flask of stream condensing unit at 1000ml, add the benzinum of 90 ~ 100 ℃ of 600g boiling points, 30g hydrogen content 1.2% molecular formula does
(CH
3)
3SiO-[(CH
3)(H)Si?O]
38.7[(CH
3)
2Si?O]
10Si(CH
3)
3
Reactant B (hydrogen molal quantity 0.36mol), the intermediate A 3 (0.06mol) of 210g embodiment 3, the a-methyl styrene reactant C (0.15mol) of 18g, the CH of 38g
2=CHC
16H
33Reactant D (0.15mol); (revolution adds the Karstedt catalyst E that accounts for system gross weight 8ppm (in platinum) 60 ~ 500r/min) times in stirring; Heating and stirring are warming up to 80 ~ 100 ℃ of back flow reaction 8h; Stir cooling then and reduce to room temperature, the check blowing must contain the petroleum ether solution (representing with G4) of 30% weight portion of special polysiloxanes.
Embodiment 9:
In the four-hole boiling flask that the 1000ml band stirs; Add DF-303 (De Fa company product solid content is 30% polyurethane resin prepolymer solution) 500g; The special polysiloxane solution G1 of 100g embodiment 5,50g white carbon flatting silica K-500 (Japanese eastern Cao company produce), 10g polyether modified siloxane levelling agent DC-193 (Dow Corning Corporation's product); 140gDMF; 100g ethyl acetate, 100g toluene stirs 30min (the cloudy surface finishing agent T1 that must contain special polysiloxanes 4.2% weight portion behind the revolution 60 ~ 500r/min).
Embodiment 10:
In the four-hole boiling flask that the 1000ml band stirs; Add DF-304 (De Fa company product solid content is 40% polyurethane resin prepolymer solution) 420g, the special polysiloxane solution G2 of 200g embodiment 6,20g polyether modified siloxane levelling agent DC-193 (Dow Corning Corporation's product); 120gDMF; 120g ethyl acetate, 120g toluene stirs 30min (bright the finishing agent T2 that must contain special polysiloxanes 9.6% weight portion behind the revolution 60 ~ 500r/min).
Embodiment 11:
In the four-hole boiling flask that the 1000ml band stirs; Add DF-303 (De Fa company product solid content is 30% polyurethane resin prepolymer solution) 400g; The special polysiloxane solution G3 of 50g embodiment 7,70g white carbon flatting silica K-500 (Japanese eastern Cao company produce), 30g polyether modified siloxane levelling agent DC-193 (Dow Corning Corporation's product); 150gDMF; 150g ethyl acetate, 150g toluene stirs 30min (the cloudy surface finishing agent T3 that must contain special polysiloxanes 3% weight portion behind the revolution 60 ~ 500r/min).
Embodiment 12:
In the four-hole boiling flask that the 1000ml band stirs; Add DF-304 (De Fa company product solid content is 40% polyurethane resin prepolymer solution) 540g, the special polysiloxane solution G4 of 150g embodiment 8,10g polyether modified siloxane levelling agent DC-193 (Dow Corning Corporation's product); 100gDMF; 100g ethyl acetate, 100g toluene stirs 30min (bright the finishing agent T4 that must contain special polysiloxanes 4.5% weight portion behind the revolution 60 ~ 500r/min).
Comparative example 1:
With embodiment 9, just willThe special polysiloxane solution G1 of 100g embodiment 5 changes the dimethyl silicone polymer toluene solution that the 100g solid content is 42% 500mpa.s into, must compare finishing agent BT-1.
Comparative example 2:
With embodiment 9,
Just willIt is 30% methyl vinyl silicone rubber toluene solution that the special polysiloxane solution G1 of 100g embodiment 5 changes the 100g solid content into, must compare finishing agent BT-2.
Comparative example 3:
With embodiment 9, just willThe special polysiloxane solution G1 of 100g embodiment 5 changes the toluene solution that the 100g solid content is 50% SP-100 (addition-type silicon rubber of the platinum complex compound catalyst system of Wa Ke company) into, must compare finishing agent BT-3.
It is following with the results list that compares finishing agent to estimate finishing agent of the present invention with the finishing agent storage stability of feel style:
Claims (4)
1. give the finishing agent of thick sliding sense style, it is characterized in that this finishing agent contains following composition: the solid content of 40 ~ 60% weight portions is 30 ~ 40% polyurethane resin prepolymer solution, the special polysiloxanes of 2 ~ 10% weight portions; The white carbon delustering agent of 0 ~ 10% weight portion; The polyether modified siloxane levelling agent of 1 ~ 3% weight portion, the DMF of 10 ~ 20% weight portions, the ethyl acetate of 10 ~ 20% weight portions; The toluene of 10 ~ 20% weight portions adds up to each component 100%;
Wherein said special polysiloxanes has following molecular formula:
Special polysiloxanes shown in the above-mentioned molecular formula is a kind of big molecule modified polyorganosiloxane that on the polysiloxanes side chain, contains long-chain dimethyl silicone polymer and aryl simultaneously or contain long-chain dimethyl silicone polymer, aryl and alkyl simultaneously; Described polyurethane resin prepolymer solution; Be meant the polyurethane resin prepolymer solution of the solid content 30 ~ 40% that forms by isocyanates and PPG or PEPA reaction that does not contain said special polysiloxanes; Be furnished with DMF, toluene, ethyl acetate, acetone or the butanols solvent of 60 ~ 70% weight portions in the solution, such polyurethane resin prepolymer solution is easy to buy from market; Described white carbon delustering agent is meant specific area 250 ~ 350m
2The precipitation method of/g or vapor phase method delustring white carbon, typical supplier and commodity have the K500 of Degussa, the N20 of watt gram, and delustering agent is easy to buy from market; Described polyether modified siloxane is meant that siloxane chain has the silicone surfactant of APEO or polyethenoxy ether or oxygen ethylene oxy propylene random copolymerization polyethers, represents commodity that DC-193 is arranged, and silicone surfactant is easy to buy from market.
2. the finishing agent of giving thick sliding sense style according to claim 1 is characterized in that: wherein, when being cloudy surface after covering with paint, lacquer, colour wash, etc., add the white carbon delustering agent of 4 ~ 10% weight portions; When being bright after covering with paint, lacquer, colour wash, etc., do not add the white carbon delustering agent.
3. the preparation method of special polysiloxanes is characterized in that this preparation method comprises following two steps in order:
One, has the preparation that a vinyl has the linear polydimethylsiloxane-intermediate A of a trimethyl silicon based end-blocking simultaneously: the vinyl pentamethyl disiloxane that in agitated reactor, adds 1 ~ 10% weight portion; The dimethyl siloxane ring body of 90 ~ 99% weight portions; 0.02 the TMAH catalyst of ~ 0.05% weight portion; Start and stir 60 ~ 500r/min, be warming up to 80 ~ 110 ℃ of reaction 2～4h, be warming up to 160～180 ℃ then; Destroy catalyst and vacuum 10～30Kpa and pull out low-boiling-point substance 1～3h, get intermediate A; Wherein, the dimethyl siloxane ring body is commodity D
3, D
4, choosing any one kind of them among the DMC; Wherein, the molecular formula of intermediate A is following:
Two, the preparation of special polysiloxanes: contain the not reactive solvents of 30 ~ 80% weight portions and the reactant of 20 ~ 70% weight portions in the preparation raw material of this special polysiloxanes; Reactive solvents is not choosing any one kind of them in the aromatic hydrocarbons, alkane, ethers, ketone, alcohols, ester class between 80 ~ 250 ℃ of the boiling points, and the reactant of 20 ~ 70% weight portions comprises following material: the vinylsiloxane intermediate A; The hydrogen containing siloxane B of hydrogen content 0.5 ~ 1.6%; The reactant C of styrene or a-methyl styrene; Molecular formula is CH
2=CH-(CH
2)
N-2The reactant D that constitutes of a-alkene (n is a positive integer, and n=8 ~ 20); The catalyst E that chooses any one kind of them in Karstedt catalyst or the speier catalyst and constitute; Wherein, the Karstedt catalyst is the platinum complex of divinyl tetramethyl disiloxane; Wherein, the speier catalyst is the aqueous isopropanol of chloroplatinic acid; Wherein, the hydrogen molal quantity of supposing the hydrogen containing siloxane B in the above-mentioned reactant of 20 ~ 70% weight portions is M
B, the molal quantity of intermediate A is M
A, the molal quantity of reactant C is M
C, the molal quantity of reactant D is M
D, M then
B: M
A: M
C: M
D=100:10 ~ 90:10 ~ 90:0 ~ 90, and (M
A+ M
C+ M
D): M
B=1 ~ 1.2:1, catalyst E account for 3 ~ 10ppm of A, B, C, D gross weight in platinum; Wherein, the molecular formula of hydrogen containing siloxane B is following:
Wherein, The preparation process of special polysiloxanes is: have heating and cooling and taking back in the reaction vessel of stream condensing unit; Add not reactive solvents and reactant A, B, C, D respectively by said ratio, stir the catalyst E that revolution 60 ~ 500r/min adds aforementioned proportion down, and stir and be warming up to 80 ~ 150 ℃ of back flow reaction 3 ~ 8h; Stir cooling then and reduce to room temperature, the check blowing gets special polysiloxane solution.
4. the preparation method of special polysiloxanes according to claim 3, it is characterized in that: wherein, the molecular weight of intermediate A is 1500 ~ 20000, degree of polymerization m=20 ~ 250.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102973863A CN102517900A (en) | 2011-09-29 | 2011-09-29 | Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102973863A CN102517900A (en) | 2011-09-29 | 2011-09-29 | Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102517900A true CN102517900A (en) | 2012-06-27 |
Family
ID=46288949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102973863A Pending CN102517900A (en) | 2011-09-29 | 2011-09-29 | Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102517900A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088644A (en) * | 2013-01-17 | 2013-05-08 | 杭州电子科技大学 | Method for preparing organosilicone modified polyether type polyurethane emulsion leather finishing agent |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59150184A (en) * | 1983-02-16 | 1984-08-28 | 三菱レイヨン株式会社 | Production of leather-like sheet with good feeling |
| EP0238991A2 (en) * | 1986-03-26 | 1987-09-30 | Bayer Ag | Coating compositions containing solvents and PU dispersions, their use in the preparation of water vapour-permeable polyurethane coatings |
| CN1693578A (en) * | 2005-05-25 | 2005-11-09 | 浙江科技学院 | Poly siloxane leather coating material and its preparation method |
| CN102174167A (en) * | 2011-02-17 | 2011-09-07 | 陈华 | Organic silicon modified polyurethane resin for synthetic leather and preparation method thereof |
| CN102199270A (en) * | 2011-04-08 | 2011-09-28 | 江苏君锐高新材料有限公司 | Polyurethane resin prepolymer solution and artificial leather fog washing bright finishing agent prepared by using same |
-
2011
- 2011-09-29 CN CN2011102973863A patent/CN102517900A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59150184A (en) * | 1983-02-16 | 1984-08-28 | 三菱レイヨン株式会社 | Production of leather-like sheet with good feeling |
| EP0238991A2 (en) * | 1986-03-26 | 1987-09-30 | Bayer Ag | Coating compositions containing solvents and PU dispersions, their use in the preparation of water vapour-permeable polyurethane coatings |
| CN1693578A (en) * | 2005-05-25 | 2005-11-09 | 浙江科技学院 | Poly siloxane leather coating material and its preparation method |
| CN102174167A (en) * | 2011-02-17 | 2011-09-07 | 陈华 | Organic silicon modified polyurethane resin for synthetic leather and preparation method thereof |
| CN102199270A (en) * | 2011-04-08 | 2011-09-28 | 江苏君锐高新材料有限公司 | Polyurethane resin prepolymer solution and artificial leather fog washing bright finishing agent prepared by using same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088644A (en) * | 2013-01-17 | 2013-05-08 | 杭州电子科技大学 | Method for preparing organosilicone modified polyether type polyurethane emulsion leather finishing agent |
| CN103088644B (en) * | 2013-01-17 | 2014-08-13 | 杭州电子科技大学 | Method for preparing organosilicone modified polyether type polyurethane emulsion leather finishing agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102167830B (en) | Process for the preparation of amine-amide-functional siloxanes | |
| CN101659671B (en) | Method for manufacturing branched sih-functional polysiloxanes and their use | |
| TW383319B (en) | Functionalized polyorganosiloxanes and one of the processes for the preparation thereof | |
| CN102382307B (en) | Bishydroxyarylsiloxane compound, method of preparing the same, and copolymer containing same | |
| CN102643565B (en) | Terminal modified organic silicone coating flatting agent and preparation method thereof | |
| CN101676318A (en) | Equilibration of siloxanes on sulphonic acid cation exchange resins containing water | |
| US5260469A (en) | Organo-siloxane with modified solubility | |
| CN102850548A (en) | Preparing organopolysiloxanes | |
| CN101910254B (en) | Polyorganosiloxane containing methacryloxy group or acryloxy group and method for producing the same | |
| CN109608640A (en) | A kind of high molecular weight MQ silicone resin and its synthetic method, application | |
| CN103642046B (en) | A kind of preparation method of end-vinyl fluorosilicon oil | |
| CN102517900A (en) | Finishing agent capable of endowing thick and smooth feel style and preparation method of special polysiloxane | |
| CA2060143C (en) | Method for the preparation of organopolysiloxane | |
| CN101560732A (en) | Modified polysiloxane softening agent and preparation method thereof | |
| CN102459078B (en) | Method for producing dodeca halogen neopentasilanes | |
| JPH04168126A (en) | Organopolysiloxane and production thereof | |
| WO2010074831A1 (en) | Preparation of siloxanes | |
| CN101220052A (en) | Method for preparing sesquialter siloxane with acid anhydride group on vertex angle | |
| CN105339417A (en) | Method for producing SiOH-functional polysiloxanes | |
| CN108707213A (en) | A kind of preparation method of hyper-branched block high-molecular copolymer and application | |
| US20050085612A1 (en) | Aminomethylene-functional siloxanes | |
| CN101092481A (en) | Acrylate group modified organic silicone when existence of rhodium catalyst | |
| JP2002508382A (en) | Production and apparatus of alkylmonohydrohalosilane by redistribution reaction and then distillation | |
| US7786241B2 (en) | Polyester silicone resins | |
| JP2715652B2 (en) | Method for producing hydrogen polysiloxane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120627 |