CN103059305B - Preparation method of antibacterial hydrophobic complexing agent for polyester fibers - Google Patents
Preparation method of antibacterial hydrophobic complexing agent for polyester fibers Download PDFInfo
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Abstract
The invention discloses a preparation method of an antibacterial hydrophobic complexing agent for polyester fibers, belonging to the field of an antibacterial agent synthetic technology. The preparation method comprises the following steps of: synthesizing carboxylpolysiloxane, wherein the carboxylpolysiloxane is generated from a hydrogen-containing saline and an acrylic acid; preparing a monoguanidyl compound, wherein the monoguanidyl compound is obtained from cyanamide and alkylamine; and carrying out condensation reaction of carboxylpolysiloxane and the monoguanidyl compound so as to obtain the antibacterial hydrophobic complexing agent. According to the invention, polysiloxane with functions of dewatering, decontaminating and the like and groups with antibacterial functions are introduced to a high polymer long chain through a way of copolymerization, so that the preparation method of the antibacterial hydrophobic complexing agent for the polyester fibers has the advantages of high efficiency, broad spectrum, good dispersibility, cheap price and the like, is free from volatility, can be easily processed at high temperature, is easy to store.
Description
Technical field
The invention belongs to antiseptic-germicide synthesis technical field, be specifically related to a kind of preparation method of trevira antibacterial hydrophobic recombiner.
Background technology
Siloxanes softening agent, the flexibility of fibre substrate, elasticity and smooth feeling can be improved for textile finishing, the good hydrophobicity of fabric and soil release performance can be given again, and through its arrange light color or white fabrics whiteness good, also have imitative numb feel, therefore have one's own knack in the stylization arrangement of fabric.
Current of a great variety of antiseptic-germicide, mainly contains five large classes, inorganic antiseptic, organic antibacterial agent, inorganic with organic composite antibiotic agent, natural antibacterial agent, polymer antibacterial agent.Silver-series antibacterial agent is oxidizable, light stability is poor, long-time uses because oxidation goods can turn black, and being on the increase, easily to environment of the heavy metal metal ion discharged in use procedure.Natural organic antibacterial agent poor heat resistance, antibacterial effect is not lasting.Polymer antiseptic-germicide to have the function monomer of anti-microbial property, and by grafting, antibacterial group is incorporated in high polymer long chain by the means such as copolymerization, and having efficient, long-acting, safe, stable etc. has good characteristic.
Summary of the invention
For prior art Problems existing, the object of the invention is to design the technical scheme of the preparation method that a kind of trevira antibacterial hydrophobic recombiner is provided.
The preparation method of described a kind of trevira antibacterial hydrophobic recombiner, is characterized in that comprising following processing step:
1) synthesis of carboxyl polysiloxane: described carboxyl polysiloxane is generated by silane containing hydrogen and vinylformic acid;
2) preparation of single guanidine compound: described single guanidine compound is generated by cyanamide and alkylamine;
3) carboxyl polysiloxane and single guanidine compound condensation reaction:
Carboxyl polysiloxane, single guanidine compound, promotor adding are equipped with in the there-necked flask of agitator, add solvent a and dissolve, be cooled to 0 ~ 5 DEG C; Slow dropping contains the solvent a of straight chain bonding reagent, is naturally warming up to room temperature, stirring reaction 2 ~ 24h, filters with solvent a washing and pressure reducing and steaming solvent a, obtains trevira antibacterial hydrophobic recombiner;
Described carboxyl polysiloxane and the molar ratio of single guanidine compound are determined according to the hydroxy radical content of carboxyl polysiloxane: n(COOH): n (single guanidine compound) is 1:1.2 ~ 1:1.5; Described straight chain bonding reagent and the molar ratio of single guanidine compound are 1.2:1 ~ 1.5:1; The molar ratio of described promotor and single guanidine compound is 1.2:1 ~ 1.5:1;
Above-mentioned straight chain bonding reagent is the one in N, N-dicyclohexylcarbodiimide, triethylamine, 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride, N, N-DIC, phosphinylidyne diimidazole;
Above-mentioned promotor is the one in I-hydroxybenzotriazole, the chloro-I-hydroxybenzotriazole of 6-, 1-hydroxyl-7-azepine benzotriazole, 4-N, N-Dimethylamino pyridine;
Above-mentioned solvent a is the one in tetrahydrofuran (THF), ethyl acetate, methylene dichloride, DMF.
The preparation method of described a kind of trevira antibacterial hydrophobic recombiner, is characterized in that the described concentration containing straight chain bonding reagent in the solvent a of straight chain bonding reagent is 1.5 ~ 5mmol/10ml.
The preparation method of described a kind of trevira antibacterial hydrophobic recombiner, is characterized in that described carboxyl polysiloxane obtains especially by following steps:
Add in the there-necked flask with agitator by silane containing hydrogen, vinylformic acid, platinum based catalyst, after stirred at ambient temperature is even, be warming up to 70 ~ 90 DEG C, reaction 20 ~ 25h terminates; Suction filtration, underpressure distillation at 50 ~ 65 DEG C of vacuum-drying 24h, obtains carboxyl silicone intermediate after removing impurity and low-boiling-point substance; Getting this intermediate appropriate is slowly added drop-wise in excessive solution b, controls rate of addition, after dropwising, reacts 1 ~ 3h and terminate at 20 ~ 40 DEG C; Be 7 by distilled water repetitive scrubbing to the pH value of washing lotion, suction filtration, at 50 ~ 65 DEG C of vacuum-drying 24h, obtains carboxyl polysiloxane;
Described silane containing hydrogen has following structure:
Wherein R
1, R
2for methyl or ethyl; R
3for H, alkyl or phenyl;
Described platinum based catalyst is the one of Platinic chloride or platinum dioxide or two kinds;
The sulphuric acid soln of described solution b to be volume fraction be 15-60%;
Described silane containing hydrogen and acrylic acid molar ratio are 1.2:1 ~ 2:1; The quality that feeds intake of platinum based catalyst is 0.01% ~ 0.05% of reactant total mass.
The preparation method of described a kind of trevira antibacterial hydrophobic recombiner, is characterized in that described single guanidine compound obtains especially by following steps:
In the there-necked flask having agitator, add alkylamine and Glacial acetic acid respectively, be warming up to 100 ~ 130 DEG C after mixing, stir and lower dropping cyanamide of bleeding, maintaining temperature of reaction is 110 ~ 130 DEG C; After dropwising, continue reaction 20 ~ 40 min, stop heating, cooling; Add the water of 2 times of volumes, heating for dissolving, with sodium hydroxide adjust ph to 10 ~ 13, leave standstill, after separating upper strata material, use the water dissolution of 2 times of volumes again, heating in water bath, carry out regulation system pH value to 7 with the acetum that Glacial acetic acid preparation quality mark is 36%, leave standstill and separate product, rotary evaporation final vacuum is dry, with solvent c recrystallization, obtain single guanidine compound.
Described cyanamide and the molar ratio of alkylamine are 1.5:1 ~ 2:1; Described Glacial acetic acid and the molar ratio of alkylamine are 1.2:1 ~ 1.5:1, and described solvent c is ethanol, chloroform or acetone.
The using method of the trevira antibacterial hydrophobic recombiner that the present invention obtains is as follows: this recombiner adds in silicone oil with the addition of 3% ~ 30%, and two roads for trevira oil operation.Within making the better infiltrated fiber top layer of described antibacterial hydrophobic recombiner, and silicone oil can covered composite yarn agent preferably, and the temperature of relaxation heat setting controls at 100 DEG C ~ 180 DEG C, and the time of relaxation heat setting is 20 ~ 40min.
Compared with prior art, positively effect of the present invention is:
Trevira antibacterial hydrophobic recombiner of the present invention will have the polysiloxane of the functions such as hydrophobic, decontamination and have antibacterial group and be incorporated in high polymer long chain by the means of copolymerization, thus have efficient, wide spectrum, non-volatile, be easy to high temperature process, favorable dispersity, be easy to plurality of advantages such as storing, cheap.
Accompanying drawing explanation
The infrared spectrum of Fig. 1 methyldiethoxysilane, vinylformic acid, carboxyl silicone intermediate and carboxyl polysiloxane;
The infrared spectrum of the mono-guanidine compound of Fig. 2;
The infrared spectrum of Fig. 3 antibacterial hydrophobic recombiner.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1: the synthesis of carboxyl polysiloxane
Get 604.125g (4.5mol) methyldiethoxysilane, 216.18g(3mol) vinylformic acid, 0.082g platinum dioxide add in the there-necked flask with agitator, stirred at ambient temperature evenly after, be warming up to 85 DEG C, reaction 23h terminates; Suction filtration, after underpressure distillation goes out decon and low-boiling-point substance, at 55 DEG C of vacuum-drying 24h, obtains carboxyl silicone intermediate; It is in the sulphuric acid soln of 40% that this intermediate getting half quality is slowly added drop-wise to excessive volume fraction, strictly controls rate of addition, after dropwising, reacts 2h and terminate at 23 DEG C; Be 7 by distilled water repetitive scrubbing to the pH value of washing lotion, suction filtration, at 55 DEG C of vacuum-drying 24h, namely obtains carboxyl polysiloxane;
Characterizing method:
Fourier transform infrared spectroscopy: liquid sample directly drips on printing opacity salt sheet, solid sample adopts pellet technique analysis, and sweep limit is 4000-400cm
-1, wherein scanning times is 32, and resolving power is 4 cm
-1.
As shown in Figure 1, the spectrogram of methyldiethoxysilane, vinylformic acid, carboxyl silicone intermediate is contrasted: 2164 cm in methyldiethoxysilane spectrogram
-1646 cm in shown Si-H stretching vibration absorption peak and vinylformic acid spectrogram
-1shown C=C unsaturated double-bond stretching vibration charateristic avsorption band, all disappears, illustrates that addition reaction of silicon with hydrogen carries out completely in the spectrogram of carboxyl silicone intermediate.
The spectrogram of contrast carboxyl polysiloxane and carboxyl silicone intermediate: 1166 cm in carboxyl silicone intermediate spectrogram
-1, 954 cm
-1the absorption peak at place disappears in the spectrogram of carboxyl polysiloxane, proves-OC
2h
5there is hydrolysis-condensation reaction.
Can be drawn by the spectrogram of carboxyl polysiloxane: 2980cm
-1there is the stretching vibration absorption peak of-OH, 1722 cm
-1occurred the stretching vibration peak of C=O double bond, these 2 demonstrate carboxyl polysiloxane and contain carboxyl; 2960 cm
-1with 2979 cm
-1for Si-CH
3middle CH
3c-H stretching vibration absorption peak, 1266 cm
-1for Si-CH
3middle CH
3symmetric vibration absorption peak, 1086-1119 cm
-1for the stretching vibration absorption peak of Si-O-Si.
In sum, the disappearance of Si-H and C=C proves that addition reaction of silicon with hydrogen carries out completely ,-OC
2h
5the disappearance of group and the appearance of Si-O-Si structure prove intermediate generation hydrolysis-condensation reaction, and the appearance of C=O and-OH illustrates that carboxyl exists, and proves that product is target product thus.
In the present invention, carboxyl polysiloxane also can be synthesized by following steps:
Get 6mol silane containing hydrogen, 3mol vinylformic acid, the Platinic chloride that accounts for reactant total mass 0.03% add in the there-necked flask with agitator, stirred at ambient temperature evenly after, be warming up to 70 DEG C, reaction 25h terminates; Suction filtration, after underpressure distillation goes out decon and low-boiling-point substance, at 50 DEG C of vacuum-drying 24h, obtains carboxyl silicone intermediate; It is in the sulphuric acid soln of 15% that this intermediate getting half quality is slowly added drop-wise to excessive volume fraction, strictly controls rate of addition, after dropwising, reacts 3h and terminate at 20 DEG C; Be 7 by distilled water repetitive scrubbing to the pH value of washing lotion, suction filtration, at 50 DEG C of vacuum-drying 24h, namely obtains carboxyl polysiloxane; Silane containing hydrogen structural formula is
Wherein R
1, R
2for methyl or ethyl; R
3for H, alkyl or phenyl.
Getting 3.6mol silane containing hydrogen, 3mol vinylformic acid, the Platinic chloride accounting for reactant total mass 0.05% and platinum dioxide adds in the there-necked flask with agitator, after stirred at ambient temperature is even, is warming up to 90 DEG C, and reaction 20h terminates; Suction filtration, after underpressure distillation goes out decon and low-boiling-point substance, at 65 DEG C of vacuum-drying 24h, obtains carboxyl silicone intermediate; It is in the sulphuric acid soln of 60% that this intermediate getting half quality is slowly added drop-wise to excessive volume fraction, strictly controls rate of addition, after dropwising, reacts 1h and terminate at 40 DEG C; Be 7 by distilled water repetitive scrubbing to the pH value of washing lotion, suction filtration, at 65 DEG C of vacuum-drying 24h, namely obtains carboxyl polysiloxane; Silane containing hydrogen structural formula is
Wherein R
1, R
2for methyl or ethyl; R
3for H, alkyl or phenyl.
Embodiment 2: the synthesis of single guanidine compound
Get 404.265g(1.5mol) stearylamine, 108.09g (1.8mol) Glacial acetic acid is in in the there-necked flask of agitator, 110 DEG C are warming up to after mixing, to stir and bleed down (water pump) drips 94.5g(2.25mol) cyanamide, maintaining temperature of reaction is 110 DEG C; After dropwising, continue reaction 30 min, stop heating, cooling; Add the water of 2 times of volumes, heating for dissolving, by sodium hydroxide adjust ph about 10, leave standstill, use the water dissolution of 2 times of volumes after separating upper strata material again, heating in water bath, carry out regulation system pH value to 7 with the acetum that Glacial acetic acid preparation quality mark is 36%, leave standstill and separate product, rotary evaporation final vacuum is dry; Single guanidine compound is obtained with ethyl alcohol recrystallization;
Characterizing method:
Fourier transform infrared spectroscopy: liquid sample directly drips on printing opacity salt sheet, solid sample adopts pellet technique analysis, and sweep limit is 4000-400 cm
-1, wherein scanning times is 32, and resolving power is 4 cm
-1.
As seen from Figure 2,1662.64 cm
-1for NH
2scissors flexural vibration absorption peak, 1620 cm
-1for the stretching vibration absorption peak of C=N, 1471cm
-1, 997 cm
-1, 770 cm
-1be respectively angle absorption peak outside the asymmetrical stretching vibration absorption peak of NCN key, symmetric vibration absorption peak and face, prove that product is target product thus.
In the present invention, single guanidine compound also can be synthesized by following steps:
Get 1mol hexadecylamine or other alkyl amine, 1.5mol Glacial acetic acid in in the there-necked flask of agitator, be warming up to 100 DEG C after mixing, to stir and bleed down (water pump) drips 2mol cyanamide, maintaining temperature of reaction is 100 DEG C; After dropwising, continue reaction 40 min, stop heating, cooling; Add the water of 2 times of volumes, heating for dissolving, by sodium hydroxide adjust ph to 13, leave standstill, use the water dissolution of 2 times of volumes after separating upper strata material again, heating in water bath, carry out regulation system pH value to 7 with the acetum that Glacial acetic acid preparation quality mark is 36%, leave standstill and separate product, rotary evaporation final vacuum is dry; With Gossypol recrystallized from chloroform, obtain single guanidine compound.
Get 1mol alkylamine, 1.3mol Glacial acetic acid in in the there-necked flask of agitator, be warming up to 130 DEG C after mixing, to stir and bleed down (water pump) drips 1.8mol cyanamide, maintaining temperature of reaction is 130 DEG C; After dropwising, continue reaction 20min, stop heating, cooling; Add the water of 2 times of volumes, heating for dissolving, by sodium hydroxide adjust ph to 12, leave standstill, use the water dissolution of 2 times of volumes after separating upper strata material again, heating in water bath, carry out regulation system pH value to 7 with the acetum that Glacial acetic acid preparation quality mark is 36%, leave standstill and separate product, rotary evaporation final vacuum is dry; With acetone recrystallization, obtain single guanidine compound.
Embodiment 3: carboxyl polysiloxane and single guanidine compound condensation reaction
The carboxyl-content being recorded carboxyl polysiloxane by acid base titration is 7.60 mmol/g;
Getting 131.58g carboxyl polysiloxane, 404.3g(1.3mol) single guanidine compound, the chloro-I-hydroxybenzotriazole of 286.57g (1.69mol) 6-(6-Cl-HOBt) add and be equipped with in the there-necked flask of agitator, add a certain amount of acetic acid ethyl dissolution, be cooled to 1 DEG C; Slow dropping contains the ethyl acetate solution (concentration of triethylamine is 2.5mmol/10ml) of 157.86g (1.56mol) triethylamine, naturally room temperature is warming up to, stirring reaction 12h, filter, by ethyl acetate washing also pressure reducing and steaming ethyl acetate, obtain trevira antibacterial hydrophobic recombiner.
Characterizing method:
Fourier transform infrared spectroscopy: liquid sample directly drips on printing opacity salt sheet, solid sample adopts pellet technique analysis, and sweep limit is 4000-400 cm
-1, wherein scanning times is 32, and resolving power is 4 cm
-1.
Can be drawn by comparison diagram 1, Fig. 2, Fig. 3: carboxyl polysiloxane infrared spectrum 2980cm in Fig. 1
-1shown in-OH stretching vibration absorption peak disappear in figure 3, single guanidine compound infrared spectrum 1662.64 cm in Fig. 2
-1shown NH
2vibration absorption peak disappear in figure 3, prove that carboxyl and guanidine radicals react thus; Carboxyl polysiloxane infrared spectrum 1086-1119 cm in Fig. 1
-1the characteristic peaks such as shown Si-O-Si stretching vibration absorption peak still exist in figure 3, single guanidine compound infrared spectrum 1620 cm in Fig. 2
-1the characteristic peaks such as shown C=N stretching vibration absorption peak still exist in figure 3, prove that product is target product.
By this recombiner with 3.5% addition add in silicone oil, two roads for trevira oil in operation.The temperature of relaxation heat setting 170 DEG C, the time of relaxation heat setting is 30min.
Succusion is adopted to measure its anti-microbial property; Utilize and adopt German Data physics company OCA40Micro model video contact angle measuring instrument to carry out contact angle test sign hydrophobic function: test under the condition of 20 DEG C, the water yield 2 μ l dripped, rate of addition 1 μ l/s, the test of static contact angle is completed in 10 s after contact, repeat 10 times, average.
Test result is shown in Table 1.
Table 1 antibacterial fiber test result
In the present invention, trevira antibacterial hydrophobic recombiner also can be obtained by following steps:
The carboxyl-content being recorded carboxyl polysiloxane by acid base titration is 7.60 mmol/g;
Get 131.58g carboxyl polysiloxane, the mono-guanidine compound of 1.2mol, 1.44 mol I-hydroxybenzotriazole (HOBt) (promotor) add and be equipped with in the there-necked flask of agitator, (solvent a) dissolves, and is cooled to 0 DEG C to add a certain amount of tetrahydrofuran (THF); Slow dropping contains 1.8mol N, (solvent is solution (N a) for the tetrahydrofuran (THF) of N-dicyclohexylcarbodiimide (DCC) (straight chain bonding reagent), the concentration of N-dicyclohexylcarbodiimide is 1.5mmol/10ml), naturally room temperature is warming up to, stirring reaction 2h, filter, with ethyl acetate washing also pressure reducing and steaming tetrahydrofuran (THF), obtain trevira antibacterial hydrophobic recombiner.
The carboxyl-content being recorded carboxyl polysiloxane by acid base titration is 7.60 mmol/g;
Get 131.58g carboxyl polysiloxane, the mono-guanidine compound of 1.5mol, 2.25mol1-hydroxyl-7-azepine benzotriazole (HOAt) or 4-N, N-Dimethylamino pyridine (DMAP) adds and is equipped with in the there-necked flask of agitator, add a certain amount of methylene dichloride to dissolve, be cooled to 5 DEG C; Slow dropping contains the dichloromethane solution (concentration of 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride is 5mmol/10ml) of 1.95mol 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride (EDCI), naturally room temperature is warming up to, stirring reaction 2h, filter, by washed with dichloromethane and pressure reducing and steaming methylene dichloride, obtain trevira antibacterial hydrophobic recombiner.
In above-described embodiment, straight chain bonding reagent can adopt N, the one in N-dicyclohexylcarbodiimide, triethylamine, 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride, N, N-DIC, phosphinylidyne diimidazole; Promotor can adopt the one in the chloro-I-hydroxybenzotriazole of I-hydroxybenzotriazole, 6-, 1-hydroxyl-7-azepine benzotriazole, 4-N, N-Dimethylamino pyridine; Solvent a can adopt the one in tetrahydrofuran (THF), ethyl acetate, methylene dichloride, DMF.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (3)
1. a trevira preparation method for antibacterial hydrophobic recombiner, is characterized in that comprising following processing step:
1) synthesis of carboxyl polysiloxane: described carboxyl polysiloxane is generated by silane containing hydrogen and vinylformic acid;
2) preparation of single guanidine compound: add alkylamine and Glacial acetic acid respectively in the there-necked flask having agitator, is warming up to 100 ~ 130 DEG C after mixing, stir and lower dropping cyanamide of bleeding, and maintaining temperature of reaction is 110 ~ 130 DEG C; After dropwising, continue reaction 20 ~ 40 min, stop heating, cooling; Add the water of 2 times of volumes, heating for dissolving, with sodium hydroxide adjust ph to 10 ~ 13, leave standstill, after separating upper strata material, use the water dissolution of 2 times of volumes again, heating in water bath, carry out regulation system pH value to 7 with the acetum that Glacial acetic acid preparation quality mark is 36%, leave standstill and separate product, rotary evaporation final vacuum is dry, with solvent c recrystallization, obtain single guanidine compound; Described cyanamide and the molar ratio of alkylamine are 1.5:1 ~ 2:1; Described Glacial acetic acid and the molar ratio of alkylamine are 1.2:1 ~ 1.5:1, and described solvent c is ethanol, chloroform or acetone;
3) carboxyl polysiloxane and single guanidine compound condensation reaction:
Carboxyl polysiloxane, single guanidine compound, promotor adding are equipped with in the there-necked flask of agitator, add solvent a and dissolve, be cooled to 0 ~ 5 DEG C; Slow dropping contains the solvent a of straight chain bonding reagent, is naturally warming up to room temperature, stirring reaction 2 ~ 24h, filters with solvent a washing and pressure reducing and steaming solvent a, obtains trevira antibacterial hydrophobic recombiner;
Described carboxyl polysiloxane and the molar ratio of single guanidine compound are determined according to the hydroxy radical content of carboxyl polysiloxane: n(COOH): n (single guanidine compound) is 1:1.2 ~ 1:1.5; Described straight chain bonding reagent and the molar ratio of single guanidine compound are 1.2:1 ~ 1.5:1; The molar ratio of described promotor and single guanidine compound is 1.2:1 ~ 1.5:1;
Above-mentioned straight chain bonding reagent is the one in N, N-dicyclohexylcarbodiimide, triethylamine, 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride, N, N-DIC, phosphinylidyne diimidazole;
Above-mentioned promotor is the one in I-hydroxybenzotriazole, the chloro-I-hydroxybenzotriazole of 6-, 1-hydroxyl-7-azepine benzotriazole, 4-N, N-Dimethylamino pyridine;
Above-mentioned solvent a is the one in tetrahydrofuran (THF), ethyl acetate, methylene dichloride, DMF.
2. the preparation method of a kind of trevira antibacterial hydrophobic recombiner as claimed in claim 1, is characterized in that the described concentration containing straight chain bonding reagent in the solvent a of straight chain bonding reagent is 1.5 ~ 5mmol/10ml.
3. the preparation method of a kind of trevira antibacterial hydrophobic recombiner as claimed in claim 1, is characterized in that described carboxyl polysiloxane obtains especially by following steps:
Add in the there-necked flask with agitator by silane containing hydrogen, vinylformic acid, platinum based catalyst, after stirred at ambient temperature is even, be warming up to 70 ~ 90 DEG C, reaction 20 ~ 25h terminates; Suction filtration, underpressure distillation at 50 ~ 65 DEG C of vacuum-drying 24h, obtains carboxyl silicone intermediate after removing impurity and low-boiling-point substance; Getting this intermediate appropriate is slowly added drop-wise in excessive solution b, controls rate of addition, after dropwising, reacts 1 ~ 3h and terminate at 20 ~ 40 DEG C; Be 7 by distilled water repetitive scrubbing to the pH value of washing lotion, suction filtration, at 50 ~ 65 DEG C of vacuum-drying 24h, obtains carboxyl polysiloxane;
Described silane containing hydrogen has following structure:
Wherein R
1, R
2for methyl or ethyl; R
3for H, alkyl or phenyl;
Described platinum based catalyst is the one of Platinic chloride or platinum dioxide or two kinds;
The sulphuric acid soln of described solution b to be volume fraction be 15-60%;
Described silane containing hydrogen and acrylic acid molar ratio are 1.2:1 ~ 2:1; The quality that feeds intake of platinum based catalyst is 0.01% ~ 0.05% of reactant total mass.
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| CN101107316A (en) * | 2005-01-28 | 2008-01-16 | 东丽株式会社 | Resin composition and fiber structural product |
| CN101273082A (en) * | 2005-08-01 | 2008-09-24 | Ge拜尔硅股份有限公司 | Polyammonium/polysiloxane copolymers |
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