Synthesis Of Silicone Water Repellent And Its Application In Textiles

The fluorine-containing water-repellent agent can give the finished fabric excellent water-repellent properties,but the problems of the fluorine-containing water-repellent agent such as refractory degradation,multi-toxicity and bioaccumulation are gradually revealed.As people's awareness of safety and environmental protection continues to increase,no fluorine The development of water repellent has very important significance.The representative one of fluorine-free water-repellent agents is organosilicon compounds,which have better biocompatibility,lower raw material prices,and can form a layer of water-repellent interface with low surface tension on the surface of the fiber.After having good water-repellent performance and a certain style of touch,it has been widely concerned by researchers and users.At present,most of the methods for researching new silicone water repellents are relatively complicated,and consume large energy and high cost,and the durability of the water repellent effect cannot be guaranteed.Therefore,the research on silicone water repellent suitable for industrial production and with good durability conforms to the development of the current era.In this project,two modified silicone water repellents were prepared,one was grafted modified silicone water repellent for finishing nylon fabrics,and one was blended modified silicone water repellent for finishing polyester fabrics.The specific research content and results are as follows:(1)With piperazine propyl methyl dimethoxysilane(GP-108),1,3-bis(aminopropyl)tetramethyldisiloxane(BAS)and octamethyl-cyclotetrasiloxane(D4)was used as the raw material and tetramethyl ammonium hydroxide(TMAH)was used as the catalyst to synthesize the amino-terminated piperazinyl polysiloxane PSO.The optimized synthesis process of PSO is:select TMAH as the catalyst and the amount(accounting for the total mass of the reaction monomer)is 0.08%,the mass ratio of the reaction monomer is m(D4):m(BAS):m(GP-108)=25:0.4:0.5,reaction temperature is 110?,reaction time is 6 h.The conversion rate of the obtained PSO was 95.3%,the ammonia value was 0.294,the viscosity was 2339 cs,and the state was a transparent,viscous liquid.Using piperazinyl polysiloxane PSO,long carbon chain acid chloride as raw material,and triethylamine(TEA)as acid binding agent,graft modified silicone water repellent GMOS was synthesized.The optimized synthesis process of GMOS is:long carbon chain acid chloride selects hexadecanoyl chloride and the mass ratio of the substance is n(primary and secondary amino):n(hexadecanoyl chloride)=1.0:1.2,the reaction temperature is 40?,the reaction time is 2 h,mixing The total amount of emulsifier(accounting for the total mass of the reaction monomer)is 20%and the mass ratio is m(1305):m(1308)=3:2.AFM,TG-DTA,FT-IR,particle size and Zeta potential,1H-NMR were used to characterize the structure and performance of GMOS.The emulsion particle size of GMOS is 120.3 nm,the Zeta potential is 37.3 mV,and the state is Translucent and bluish blue.The modified nylon fabric with grafted modified silicone water-repellent agent GMOS is used.The optimized finishing process of GMOS is:a finishing solution with a concentration of 120 g/L and a pH of 6-7.It is baked at 180? for 1.5 min.After finishing with GMOS,the nylon fabric The water repellent grade is 90 points,the contact angle is 129.3°,the mean coefficient of dynamic friction(MIU)and surface roughness(SMD)of the latitude and longitude directions are slightly decreased,and the bending stiffness(B)and bending hysteresis moment(2HB)of the latitude and longitude directions are obvious Decreased,the compression specific work(WC)and compression resilience(RC)increased significantly.After finishing,the nylon fabric has a fluffy and soft style feel;the breaking strength,breathability and whiteness decreased slightly,the yellowing value increased slightly,GMOS After being washed 15 times,the finished nylon fabric has a water-repellent rating of 80 points an da contact angle of 111.7°.The MIU,SMD,B,2HB,WC,and RC in the latitude and longitude directions do not change much,and the breaking strength,breathability,whiteness and The yellowing value does not change much,indicating that the GMOS molecule has good washing resistance on the nylon fabric.(2)Double-terminal epoxy polysiloxane was synthesized using epoxy double-sealed head(MTMS),octamethyl-cyclotetrasiloxane(D4)as raw material,and tetramethylammonium hydroxide(TMAH)as catalyst.EPSO.The optimized synthesis process of EPSO is:the mass ratio of the reaction monomer is n(MTMS):n(D4)=0.8:20,the reaction time is 6h,and the reaction temperature is 95?.The viscosity of the obtained EPSO was 2250 cs,and the epoxy retention rate was 96.9%.Hyper-branched piperazinyl polysiloxane HPSO was synthesized using EPSO and 1,4-bis(3-aminopropyl)piperazine(BAPP)as the raw materials.The optimized synthesis process of HPSO is:the mass ratio of the reacted monomer is n(EPSO):n(BAPP)=2:1,the reaction time is 6h,and the reaction temperature is 80?.The viscosity of the obtained HPSO is 2790 cs,the state is yellow and transparent.The hyperbranched piperazinyl polysiloxane HPSO was characterized by FT-IR,1H-NMR and TG-DTA.Using hyperbranched piperazinyl polysiloxane HPSO and hydrogen-containing polysiloxane(PHMS)as raw materials,1303,1305,1308and 1227 as emulsifiers,the blended modified silicone water repellent BMOS was obtained.The optimized blending process of BMOS is:the viscosity of hydrogen-containing polysiloxane(PHMS)is 800?1000 cs,the blending ratio of raw materials is m(HPSO):m(PHMS)=1:1,the total amount of mixed emulsifier(Accounting for the total mass of the blended raw materials)is 30%and the ratio is m(1303):m(1305):m(1308):m(1227)=2:2.4:1,6:0.6,and the emulsification temperature is 50?,The emulsification time is 1h.The performance of BMOS is characterized.The emulsion particle size of BMOS is 216.8 nm,the Zeta potential is 26.7 mV,and the state is milky white and bluish blue.The polyester fabric is finished with blended modified silicone water repellent BMOS.The optimized finishing process of BMOS is:a finishing solution with a concentration of 80 g/L and a pH value of 5?6,baked at 160? for 1.5 min,and finished with BMOS.The fabric has a water-repellent rating of 90 points and a contact angle of 130.1°.The mean coefficient of dynamic friction(MIU)and surface roughness(SMD)in the warp and weft directions are significantly reduced,and the bending stiffness(B)and bending hysteresis in the warp and weft directions(2HB)Decrease,the compression ratio work(WC)and compression resilience(RC)increase slightly.After finishing,the polyester fabric has a certain degree of softness and smoothness.The breaking strength,air permeability and whiteness decrease slightly,and the yellowing value increases slightly.BMOS-treated polyester fabric has a water-repellent rating of 80 points after being washed 15 times and a contact angle of 116.3°.The MIU,SMD,B,2HB,WC,and RC in the latitude and longitude directions have little change,and the breaking strength,breathability,and whiteness The yellowing value does not change much,indicating that the BMOS molecule has good washing resistance on polyester fabrics.