CN101550659B - A silica gel used for loomage coating and silk screen printing and preparing method thereof - Google Patents
A silica gel used for loomage coating and silk screen printing and preparing method thereof Download PDFInfo
- Publication number
- CN101550659B CN101550659B CN2009101433023A CN200910143302A CN101550659B CN 101550659 B CN101550659 B CN 101550659B CN 2009101433023 A CN2009101433023 A CN 2009101433023A CN 200910143302 A CN200910143302 A CN 200910143302A CN 101550659 B CN101550659 B CN 101550659B
- Authority
- CN
- China
- Prior art keywords
- silica gel
- preparation
- agent
- silk
- shares
- 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.)
- Expired - Fee Related
Links
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a silica gel used for loomage coating and silk screen printing, which includes the components of the following weight proportion: elements gum 92-98 shares and dummy honour additive 2-5 shares. The elements gum includes polysiloxane linear body 70-80 shares, strengthening filling agent 20-30 shares, and additive 1-5 shares, the additive includes bridging agent 0.1-0.3 shares, cross linker 1-5 shares and inhibitor 0.02-0.05 shares. The surface of the aforementioned silica gel takes dummy honour effect after flatted and cured on the loomage, which makes the characters or patterns on the silica gel clear to be distinguished, and is propitious for user to identify the appellation and brand of the grubstake from long distance. The invention still provides a method for preparing the aforementioned silica gel, which concretely includes the following steps: 1) preparing elements gum, 2) preparing dummy honour additive, 3) preparing the dummy honour silica gel used for loomage coating and silk screen printing. The aforementioned preparing method can be used into the existing industrial raw materials and implements high yield of the final products with simple operationsteps and large-scale producing.
Description
Technical field
The invention belongs to the material field, specifically relate to a kind of mute light silica gel that is used for fabric coating and silk-screen and preparation method thereof.
Background technology
Organic-silicon-modified technical development to existing rubber is maked rapid progress, and various organic-silicon-modified rubber emerge in an endless stream.For example, the research of organic silicon modified polyurethane, method of modifying has modification by copolymerization, it also can be blending and modifying, organosilicon modifier mainly contains silane (as KH-550, KH-560) or polysiloxanes (as hydroxy silicon oil, amido silicon oil), and modified product is mainly as adhesive, coating, epoxy resin toughener, textile coating agent; Fluoroalkyl modified silicon oil and emulsion thereof with waterproof and oilproof function are mainly as fabric finishing agent and lubricating oil; By hydrosilylation allyl polyethenoxy polyethenoxy ether, fluorinated acrylamide acid alkyl ester are grafted to the Methyl Hydrogen Polysiloxane Fluid side chain, have synthesized a series of water-based silicon-fluorine polymer things.
Though existing organic-silicon-modified silica gel is of a great variety, the alternative scope of add-on type liquid organosilicon rubber that is used for fabric coating and silk-screen is very wide, but, the existing add-on type liquid organosilicon rubber of fabric coating and silk-screen that is used for is after levelling on the textiles solidifies, the surface is wet look, at some the product of mute light requirement is arranged, just need exploitation and composition to solidify the silica gel that the rear surface is mute light effect.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of mute light silica gel that is used for fabric coating and silk-screen and preparation method thereof is provided.
The present invention solves the problems of the technologies described above the technical scheme that is adopted to be:
A kind of silica gel that is used for fabric coating and silk-screen, it comprises the component of following weight portion: 2～5 parts of 92～98 parts in basic glue and mute light auxiliary agents, this basis glue comprises 1～5 part of 70～80 parts of polysiloxanes linear bodies, 20～30 parts of reinforced fillings and auxiliary agent, and this auxiliary agent comprises 0.02～0.05 part in 0.1～0.3 part of bridging agent, 1～5 part of crosslinking agent and inhibitor.
A kind of silica gel that is used for fabric coating and silk-screen, described basic glue is add-on type liquid organosilicon glue, and described mute light auxiliary agent is N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, and described reinforced filling is a white carbon, described bridging agent is a platinum complex, and described crosslinking agent is a containing hydrogen silicone oil.
A kind of silica gel that is used for fabric coating and silk-screen, described bridging agent are platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both, described inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.
A kind of silica gel that is used for fabric coating and silk-screen, described containing hydrogen silicone oil are linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of wherein said a is 1～2, the span of described b is 2～8.
The preparation method of the above-mentioned silica gel that is used for fabric coating and silk-screen, it specifically comprises the steps:
1. the preparation of basic glue
1) preparation of base polymer: with dimethyl siloxane mixture (DMC) is raw material, obtains having the polydiorganosiloxanepolyurea of vinyl through the base catalysis ring-opening polymerization, and its reaction equation is as follows:
2) preparation of reinforced filling: white carbon is handled under finishing agent, obtained the fume colloidal silica that specific area is 150-400;
3) get the base polymer and the step 2 of 70～80 weight portions of step 1) preparation) reinforced filling of 20～weight portion of preparation puts into kneader, mix after 3～6 hours, under 140 ℃～180 ℃, vacuumize and remove low-boiling point material, the cooling back adds the bridging agent of 0.1～0.3 weight portion, obtains mixture A;
4) inhibitor of 1～5 parts by weight of cross-linking agent and 0.02～0.05 weight portion is stirred after, obtain mixture B;
5) after mixture A that above-mentioned steps is prepared and mixture B fully mix, be warming up to 100 ℃～120 ℃, keep this temperature 3min～15min, be sulfided into solid, make basic glue until mixture;
2. the preparation of mute light auxiliary agent
1) being raw material with dimethyl dichlorosilane (DMCS) and allyl chloride, is catalyst with the chloroplatinic acid, by hydrosilylation, and synthetic intermediate (I): methyl (γ-chloropropyl) dichlorosilane;
2) alcoholysis reaction: above-mentioned intermediate (I) is dropped in three mouthfuls of round-bottomed flasks; load onto constant pressure funnel and reflux condensing tube; the absolute methanol of in constant pressure funnel, packing into; under nitrogen protection, be heated to 80 ℃～120 ℃; in 40min, drip methyl alcohol, react 2～6h again, first air-distillation; steam fraction below 110 ℃, 2.7 * 10
3Fraction between decompression distillation is collected 88～92 ℃ under the Pa, the liquid that obtains is intermediate (II);
3) aminolysis reaction: in there-necked flask, add ethylenediamine, load onto reflux condensing tube and constant pressure funnel, after in constant pressure funnel, adding intermediate (II), begin to stir, under nitrogen protection, be heated to 130 ℃～160 ℃, drip intermediate (II) at 20min～40min, react 1-6h after dripping off again; Post reaction mixture is changed in the separatory funnel, and static, system is divided into two-layer, and the upper strata is thick product, and lower floor is ethylenediamine and hydrochloride thereof, divides sub-cloud, with supernatant liquid 3.33 * 10
3Decompression distillation under the Pa, the fraction between collecting 139～141 ℃, the liquid that obtains are mute light auxiliary agent: N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane;
Above-mentioned steps 1), 2) and 3) in the chemical equation of reaction as follows:
3. be used for the preparation of the mute light silica gel of fabric coating and silk-screen
At coefficient of viscosity is in the basic glue of 92～98 weight portions of 100PS～600PS, adds the mute light auxiliary agent of 2～5 weight portions, after stirring, promptly makes the mute light silica gel that is used for fabric coating and silk-screen.
The preparation method of the above-mentioned silica gel that is used for fabric coating and silk-screen, the boiling range of described intermediate (I) are 186 ℃～188 ℃, and index of refraction is n25D:1.4596, and gas chromatographic purity is 98.4%.
The preparation method of the above-mentioned silica gel that is used for fabric coating and silk-screen, the concrete preparation process of described reinforced filling is: 1. prepare finishing agent: add the dimethyldimethoxysil,ne of 15～30 weight portions and the dimethyldiethoxysilane of 15～30 weight portions in the HMDS of 60 weight portions; 2. with Bai Tan ?and finishing agent put into reactor jointly and mix, be warming up to 80 ℃～120 ℃ then, under 2-5 atmospheric condition, handled 4～6 hours, obtain specific area and be 150～400 vapor phase method Bai Tan ?, the silica gel material that the reinforced filling of handling is in this way made improves a lot on tearing toughness and percentage elongation.
The mute light silica gel that is used for fabric coating and silk-screen of above-mentioned preparation, its mute light principle is: utilize the thixotroping of mute light auxiliary agent to the silica gel fluid, destroy the flowability of liquid-state silicon gel, the even site and the fiber vestige in length and breadth of its colloid surface after being screen-printed on the textiles are preserved, make light shine rough surface and form diffuse scattering, form mute light effect.
Beneficial effect of the present invention is: the mute light silica gel that is used for fabric coating and silk-screen provided by the invention, it is after levelling on the fabric solidifies, the surface presents mute light effect, thereby font or clear patterns on the silica gel can be distinguished, helps the buyer and recognizes clothes title and brand at a distance; The preparation method who is used for the mute light silica gel of fabric coating and silk-screen provided by the invention, it can use the high yield that the existing raw material of industry is realized finished product, and operating procedure is simple, carries out large-scale production easily.
The specific embodiment
Embodiment 1: the silica gel that is used for fabric coating and silk-screen that present embodiment provides, it comprises two parts: basic glue and mute light auxiliary agent, the shared part by weight of each component is: 3 parts of 92 parts in basic glue and mute light auxiliary agents, this basis glue comprises 2 parts of 70 parts of polysiloxanes linear bodies, 20 parts of reinforced fillings and auxiliary agents, and this auxiliary agent comprises 0.02 part in 0.1 part of bridging agent, 2 parts of crosslinking agents and inhibitor.In the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both, crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.
Present embodiment also provides a kind of preparation method who is used for the mute light silica gel of fabric coating and silk-screen, it comprises basic glue and mute light auxiliary agent, this basis glue comprises base polymer, reinforced filling and auxiliary agent, auxiliary agent comprises bridging agent, crosslinking agent and inhibitor, in the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2And Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH], crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of wherein said a is 1, and the span of described b is 3, and described inhibitor is 3-methyl isophthalic acid-butine-3-alcohol, and its concrete making step is as follows:
1. the preparation of basic glue
1) preparation of base polymer: with dimethyl siloxane mixture (DMC) is raw material, obtains having the polydiorganosiloxanepolyurea of vinyl through the base catalysis ring-opening polymerization, and its reaction equation is as follows:
2) preparation of reinforced filling: 1. prepare finishing agent: in the HMDS of 60 weight portions, add the dimethyldimethoxysil,ne of 15～30 weight portions and the dimethyldiethoxysilane of 15～30 weight portions; 2. with the Bai Tan of above-mentioned steps preparation ?and finishing agent put into reactor jointly and mix, be warming up to 120 ℃ then, under 3 atmospheric conditions, handled 4～6 hours, obtain specific area and be 300 vapor phase method Bai Tan ?.
3) get the base polymer and the step 2 of 80 weight portions of step 1) preparation) reinforced filling of 20 weight portions of preparation puts into kneader, mix after 3～6 hours, under 160 ℃, vacuumize and remove low-boiling point material, the cooling back adds the bridging agent of 0.1 weight portion, obtains mixture A;
4) inhibitor of 2 parts by weight of cross-linking agent and 0.02 weight portion is stirred after, obtain mixture B:
5) behind the mixture A and mixture B mixing with the above-mentioned steps preparation, be warming up to 100 ℃～120 ℃, keep this temperature a period of time, be sulfided into solid, make basic glue until mixture;
2. the preparation of mute light auxiliary agent
1) be raw material with dimethyl dichlorosilane (DMCS) and allyl chloride, with the chloroplatinic acid is catalyst, pass through hydrosilylation, synthetic intermediate (I): methyl (γ-chloropropyl) dichlorosilane, the yield of this intermediate (I) is 80.94%, its performance parameter is: boiling range: 186～188 ℃, and index of refraction n25D:1.4596, gas chromatographic purity is 98.4%.
2) alcoholysis reaction: the intermediate (I) of 80 weight portions is dropped in three mouthfuls of round-bottomed flasks; load onto constant pressure funnel and reflux condensing tube; in constant pressure funnel, pack into the absolute methanol of 20 weight portions; under nitrogen protection, be heated to 80 ℃～120 ℃; in 40min, drip methyl alcohol, react 2～6h again after, with the mixture air-distillation that obtains; steam fraction below 110 ℃, 2.7 * 10
3Decompression distillation under the Pa, the fraction between collecting 88～92 ℃ is intermediate (II).The purity gas chromatographic analysis of intermediate (II).
3) aminolysis reaction: the ethylenediamine that in there-necked flask, adds weight 60 weight portions, load onto reflux condensing tube and constant pressure funnel, after in constant pressure funnel, adding the intermediate (II) of 40 weight portions, begin to stir, under nitrogen protection, be heated to 130 ℃～160 ℃, in 0.5h, drip intermediate (II), drip off the back and react 2～6h again by setting; Material is changed in the separatory funnel, static, system is divided into two-layer, the upper strata is a product, and lower floor is ethylenediamine and hydrochloride thereof, divides sub-cloud, with supernatant liquid decompression distillation under 3.33 * 103Pa, fraction between collecting 139～141 ℃ promptly obtains mute light auxiliary agent: N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, its purity aceticanhydride drips of solution setting analysis of perchloric acid.
Step 1), 2) and 3) in the chemical equation of reaction as follows:
3. be used for the preparation of the mute light silica gel of fabric coating and silk-screen
At coefficient of viscosity is in the basic glue of 92 weight portions of 200PS, the mute light auxiliary agent that adds 3 weight portions, after stirring, promptly make the mute light silica gel that is used for fabric coating and silk-screen, this mute light silica gel that is used for fabric coating and silk-screen is curable at fabric in design temperature and setting-up time.
Embodiment 2: the silica gel that is used for fabric coating and silk-screen that present embodiment provides, it comprises two parts: basic glue and mute light auxiliary agent, the shared part by weight of each component is: 2 parts of 96 parts in basic glue and mute light auxiliary agents, this basis glue comprises 3 parts of 75 parts of polysiloxanes linear bodies, 25 parts of reinforced fillings and auxiliary agents, and this auxiliary agent comprises 0.04 part in 0.2 part of bridging agent, 3 parts of crosslinking agents and inhibitor.In the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both, crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of wherein said a is 1.5, and the span of described b is 5, and inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.
Present embodiment also provides a kind of preparation method who is used for the mute light silica gel of fabric coating and silk-screen, it comprises basic glue and mute light auxiliary agent, this basis glue comprises base polymer, reinforced filling and auxiliary agent, auxiliary agent comprises bridging agent, crosslinking agent and inhibitor, in the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2And Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH], crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.Concrete making step is as follows:
1. the preparation of basic glue
1) preparation of base polymer: with dimethyl siloxane mixture (DMC) is raw material, obtains having the polydiorganosiloxanepolyurea of vinyl through the base catalysis ring-opening polymerization, and its reaction equation is as follows:
2) preparation of reinforced filling: 1. prepare finishing agent: in the HMDS of 60 weight portions, add the dimethyldimethoxysil,ne of 22 weight portions and the dimethyldiethoxysilane of 30 weight portions; 2. with Bai Tan ?and finishing agent put into reactor jointly and mix, be warming up to 120 ℃ then, under 3 atmospheric conditions, handled 4～6 hours, obtain specific area and be 150 vapor phase method Bai Tan ?, the silica gel material that the reinforced filling of handling is in this way made improves a lot on tearing toughness and percentage elongation.
3) get the base polymer and the step 2 of 80 weight portions of step 1) preparation) reinforced filling of 25 weight portions of preparation puts into kneader, mix after 3～6 hours, under 160 ℃, vacuumize and remove low-boiling point material, the cooling back adds the bridging agent of 0.2 weight portion, obtains mixture A;
4) inhibitor of 2 parts by weight of cross-linking agent and 0.08 weight portion is stirred after, obtain mixture B;
5) behind the mixture A and mixture B mixing with the above-mentioned steps preparation, be warming up to 100 ℃～120 ℃, keep this temperature a period of time, be sulfided into solid, make basic glue until mixture;
2. the preparation of mute light auxiliary agent, its basic step is with embodiment 1.
3. be used for the preparation of the mute light silica gel of fabric coating and silk-screen
At coefficient of viscosity is in the basic glue of 96 weight portions of 300PS, the mute light auxiliary agent that adds 2 weight portions, after stirring, promptly make the mute light silica gel that is used for fabric coating and silk-screen, this mute light silica gel that is used for fabric coating and silk-screen is curable at fabric in design temperature and setting-up time.
Embodiment 3: the silica gel that is used for fabric coating and silk-screen that present embodiment provides, it comprises two parts: basic glue and mute light auxiliary agent, the shared part by weight of each component is: 5 parts of 98 parts in basic glue and mute light auxiliary agents, this basis glue comprises 5 parts of 80 parts of polysiloxanes linear bodies, 30 parts of reinforced fillings and auxiliary agents, and this auxiliary agent comprises 0.05 part in 0.3 part of bridging agent, 5 parts of crosslinking agents and inhibitor.In the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both, crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of wherein said a is 2, and the span of described b is 8, and described inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.
Present embodiment also provides a kind of preparation method who is used for the mute light silica gel of fabric coating and silk-screen, it comprises basic glue and mute light auxiliary agent, this basis glue comprises base polymer, reinforced filling and auxiliary agent, auxiliary agent comprises bridging agent, crosslinking agent and inhibitor, in the present embodiment, bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2And Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH], crosslinking agent is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, inhibitor is 3-methyl isophthalic acid-butine-3-alcohol.Concrete making step is as follows:
1. the preparation of basic glue
1) preparation of base polymer: with dimethyl siloxane mixture (DMC) is raw material, obtains having the polydiorganosiloxanepolyurea of vinyl through the base catalysis ring-opening polymerization, and its reaction equation is as follows:
2) preparation of reinforced filling: 1. prepare finishing agent: in the HMDS of 60 weight portions, add the dimethyldimethoxysil,ne of 30 weight portions and the dimethyldiethoxysilane of 25 weight portions; 2. with Bai Tan ?and finishing agent put into reactor jointly and mix, be warming up to 120 ℃ then, under 3 atmospheric conditions, handled 4～6 hours, obtain specific area and be 400 vapor phase method Bai Tan ?, the silica gel material that the reinforced filling of handling is in this way made improves a lot on tearing toughness and percentage elongation.
3) get the base polymer and the step 2 of 80 weight portions of step 1) preparation) reinforced filling of 30 weight portions of preparation puts into kneader, mix after 3～6 hours, under 160 ℃, vacuumize and remove low-boiling point material, the cooling back adds the bridging agent of 0.3 weight portion, obtains mixture A;
4) inhibitor of 2 parts by weight of cross-linking agent and 0.2 weight portion is stirred after, obtain mixture B;
5) behind the mixture A and mixture B mixing with the above-mentioned steps preparation, be warming up to 100 ℃～120 ℃, keep this temperature a period of time, be sulfided into solid, make basic glue until mixture;
2. the preparation of mute light auxiliary agent, its basic step is with embodiment 1.
3. be used for the preparation of the mute light silica gel of fabric coating and silk-screen
At coefficient of viscosity is in the basic glue of 98 weight portions of 600PS, the mute light auxiliary agent that adds 5 weight portions, after stirring, promptly make the mute light silica gel that is used for fabric coating and silk-screen, this mute light silica gel that is used for fabric coating and silk-screen is curable at fabric in design temperature and setting-up time.
Experimental raw and instrument: the used main raw material of above-mentioned steps is commercial grade, and purifying does not directly use.Dimethyl dichlorosilane (DMCS) (purity 98.2%) wherein, allyl chloride (purity 98.5%), absolute methanol and anhydrous ethylenediamine are commercially available industrial goods, other medicine such as chloroplatinic acid is a chemically pure reagent.Detecting instrument is a gas chromatograph.
The present invention is not limited to above-mentioned embodiment, and every all embodiments that are equal to that can realize the object of the invention are all within protection scope of the present invention.
Claims (5)
1. a silica gel that is used for fabric coating and silk-screen is characterized in that, it comprises the component of following weight portion: 2～5 parts of 92～98 parts in basic glue and mute light auxiliary agents; Should basis glue be add-on type liquid organosilicon glue wherein, it comprises 1～5 part of 70～80 parts of polysiloxanes linear bodies, 20～30 parts of reinforced fillings and auxiliary agent, this auxiliary agent comprises 0.02～0.05 part in 0.1～0.3 part of bridging agent, 1～5 part of crosslinking agent and inhibitor, and wherein bridging agent is platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both, crosslinking agent is a containing hydrogen silicone oil, inhibitor is 3-methyl isophthalic acid-butine-3-alcohol, reinforced filling is a white carbon; Described mute light auxiliary agent is N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane.
2. the silica gel that is used for fabric coating and silk-screen according to claim 1 is characterized in that, described containing hydrogen silicone oil is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of wherein said a is 1～2, the span of described b is 2～8.
3. the described preparation method who is used for the silica gel of fabric coating and silk-screen of claim 1 is characterized in that it specifically comprises the steps:
1. the preparation of basic glue
1) preparation of base polymer: with the dimethyl siloxane mixture is raw material, obtains having the polydiorganosiloxanepolyurea of vinyl through the base catalysis ring-opening polymerization, and its reaction equation is as follows:
2) preparation of reinforced filling: white carbon is handled under finishing agent, obtained the fume colloidal silica that specific area is 150-400;
3) get the base polymer and the step 2 of step 1) preparation) after the reinforced filling of preparation fully mixes 3～6 hours, under 140 ℃～180 ℃, vacuumize and remove low-boiling point material, the cooling back adds bridging agent, obtains mixture A; Bridging agent wherein is platinum group catalyst Pt[(ViMe
2Si)
2O]
2Or Pt[(ViMe
2Si)
2O] [ViMe
2SiOSiMe
2OH] in one or both;
4) crosslinking agent and inhibitor are stirred after, obtain mixture B; Crosslinking agent wherein is linear methyl hydrogen silicone oil Me
2SiO (Me
2SiO)
a(MeHSiO)
bSiMe
2, the span of its a is 1～2, the span of b is 2～8; Inhibitor is 3-methyl isophthalic acid-butine-3-alcohol;
5) after mixture A that above-mentioned steps is prepared and mixture B fully mix, be warming up to 100 ℃～120 ℃, keep this temperature 3min～15min, be sulfided into solid, make basic glue until mixture;
2. the preparation of mute light auxiliary agent
1) being raw material with dimethyl dichlorosilane (DMCS) and allyl chloride, is catalyst with the chloroplatinic acid, by hydrosilylation, and synthetic intermediate (I): methyl (γ-chloropropyl) dichlorosilane;
2) alcoholysis reaction: above-mentioned intermediate (I) is dropped in three mouthfuls of round-bottomed flasks; load onto constant pressure funnel and reflux condensing tube; the absolute methanol of in constant pressure funnel, packing into; under nitrogen protection, be heated to 80 ℃～120 ℃; in 40min, drip methyl alcohol, react 2～6 hours again after, with the mixture air-distillation that obtains; steam fraction below 110 ℃, 2.7 * 10
3Fraction between decompression distillation is collected 88～92 ℃ under the Pa, the liquid that obtains is intermediate (II);
3) aminolysis reaction: in there-necked flask, add ethylenediamine, load onto reflux condensing tube and constant pressure funnel, in constant pressure funnel, add intermediate (II) after, begin to stir,
N2Be heated to 130 ℃～160 ℃ under the protection, drip intermediate (II), react 1-6h after dripping off again at 20min～40min; Post reaction mixture is changed in the separatory funnel, and static, system is divided into two-layer, and the upper strata is thick product, and lower floor is ethylenediamine and hydrochloride thereof, divides sub-cloud, with supernatant liquid 3.33 * 10
3Decompression distillation under the Pa, the fraction between collecting 139～141 ℃, the liquid that obtains are mute light auxiliary agent: N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane;
Above-mentioned steps 1), 2) and 3) in the chemical equation of reaction as follows:
3. be used for the preparation of the mute light silica gel of fabric coating and silk-screen
At coefficient of viscosity is in the basic glue of 100PS～600PS, adds mute light auxiliary agent, after stirring, promptly makes the mute light silica gel that is used for fabric coating and silk-screen.
4. the preparation method who is used for the silica gel of fabric coating and silk-screen according to claim 3 is characterized in that, the boiling range of described intermediate (I) is 186 ℃～188 ℃, and index of refraction is n25D:1.4596, and gas chromatographic purity is 98.4%.
5. the preparation method who is used for the silica gel of fabric coating and silk-screen according to claim 4, it is characterized in that, the concrete preparation process of described reinforced filling is: 1. prepare finishing agent: 2. the dimethyldiethoxysilane that adds the dimethyldimethoxysil,ne of 15～30 weight portions and 15～30 weight portions in the HMDS of 60 weight portions is put into white carbon and finishing agent jointly reactor and is mixed and be warming up to 80 ℃～120 ℃ then, under 2-5 atmospheric condition, handled 4～6 hours, and obtained specific area and be 150～400 fume colloidal silica.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101433023A CN101550659B (en) | 2009-05-19 | 2009-05-19 | A silica gel used for loomage coating and silk screen printing and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101433023A CN101550659B (en) | 2009-05-19 | 2009-05-19 | A silica gel used for loomage coating and silk screen printing and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101550659A CN101550659A (en) | 2009-10-07 |
| CN101550659B true CN101550659B (en) | 2011-06-29 |
Family
ID=41155131
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101433023A Expired - Fee Related CN101550659B (en) | 2009-05-19 | 2009-05-19 | A silica gel used for loomage coating and silk screen printing and preparing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101550659B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798391B (en) * | 2010-03-29 | 2012-03-21 | 东莞市良展有机硅科技有限公司 | Process for preparing modified textile silica gel and product thereof |
| CN103031748B (en) * | 2012-12-31 | 2015-05-20 | 江苏天辰新材料有限公司 | Single-component heat-curing silk-screen printing silica gel and preparation method thereof |
| CN105602444B (en) * | 2016-03-07 | 2018-05-15 | 惠州赛力珑新材料有限公司 | A kind of Yoga mat and preparation method |
| CN106674525A (en) * | 2017-01-18 | 2017-05-17 | 东莞市港田高分子材料有限公司 | Production method of matte silk-printing silica gel |
| CN106917306B (en) * | 2017-04-13 | 2021-01-08 | 广东省良展有机硅科技有限公司 | Priming printing silica gel for elliptical machine and preparation method thereof |
| CN107637896A (en) * | 2017-09-14 | 2018-01-30 | 昆山腾飞内衣科技股份有限公司 | The preparation method of semi-aqueous silica gel, dress ornament and the dress ornament |
| CN108049225A (en) * | 2017-11-29 | 2018-05-18 | 东莞市良展有机硅科技有限公司 | The preparation method of textile multi color printing coating and the multi color printing coating |
| CN108425247B (en) * | 2018-04-17 | 2019-04-19 | 南通全技纺织涂层有限公司 | Reduce the silica gel and preparation method thereof of fabric seam sliding |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106673A (en) * | 1984-07-26 | 1987-03-25 | 钟渊化学工业株式会社 | Curable polymeric composition |
| US6140414A (en) * | 1998-07-16 | 2000-10-31 | Shin-Etsu Chemical Co., Ltd. | Aqueous silicone emulsion and base cloth for air bags treated therewith |
| CN1813026A (en) * | 2003-07-08 | 2006-08-02 | 株式会社钟化 | Curing composition |
-
2009
- 2009-05-19 CN CN2009101433023A patent/CN101550659B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106673A (en) * | 1984-07-26 | 1987-03-25 | 钟渊化学工业株式会社 | Curable polymeric composition |
| US6140414A (en) * | 1998-07-16 | 2000-10-31 | Shin-Etsu Chemical Co., Ltd. | Aqueous silicone emulsion and base cloth for air bags treated therewith |
| CN1813026A (en) * | 2003-07-08 | 2006-08-02 | 株式会社钟化 | Curing composition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101550659A (en) | 2009-10-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101550659B (en) | A silica gel used for loomage coating and silk screen printing and preparing method thereof | |
| CN1075526C (en) | Organosilicone having a carboxyl functional group thereon | |
| CN101891959B (en) | Addition-curable silicone composition for providing cured product having high refractive index and optical element encapsulating material comprising the same | |
| CN101300305B (en) | Curable organic silicone composition | |
| EP2392608B1 (en) | Method for producing organic silicon compounds | |
| CN110305486A (en) | A kind of silicon gel and preparation method thereof | |
| US20130213267A1 (en) | Composition Comprising Polymers and Metal Atoms or Ions and Use Thereof | |
| CN102898649B (en) | Refractive index-adjustable MDT silicone resin and preparation method thereof | |
| CN100457803C (en) | Fluoric alkoxyl propyl methyl silicone oil and its prepn process | |
| CN107540843A (en) | The function additive of side base containing chain alkyl and epoxy based polysiloxane and preparation method thereof | |
| CN107312496B (en) | Adhesive addition type liquid silicone rubber | |
| CN103848991A (en) | Organosilicon gel emulsion for daily chemicals, and preparation method and applications thereof | |
| CN101781328A (en) | Preparation method of cyclosiloxane | |
| CN101230073B (en) | Method for preparing phenyl-containing mixed cyclic siloxane | |
| CN105218822A (en) | Phenyl hydrogen-containing silicon oil of LED liquid-packing glue and preparation method thereof is rolled over for height | |
| CN102844321B (en) | Silicon polyethers and preparation method thereof | |
| CN109679350A (en) | A kind of optical grade silica gel for optical device | |
| CN109689734B (en) | Method for continuously producing low alkoxy branched siloxane | |
| CN107674639A (en) | A kind of preparation method of organosilicon adhesive | |
| CN104356391B (en) | The synthetic method of high-vinyl-content vinyl phenyl silicone oil | |
| Elmanovich et al. | Silicone aerogels with tunable mechanical properties obtained via hydrosilylation reaction in supercritical CO2 | |
| CN114196215B (en) | MTQ silicone resin, preparation method thereof, fluorine-containing organic silicone rubber, preparation method thereof and application thereof | |
| JP6991355B2 (en) | Method for preparing oxamide functional siloxane | |
| CN106986890A (en) | A kind of environment-friendly preparation method of the pentamethyl cyclotrisiloxane of 2 vinyl 2,4,4,6,6 | |
| CN103204994A (en) | Preparation method of phenyl silicon resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110629 Termination date: 20190519 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |