| Amino-silicone oil finishing agent gives cotton fabric not only excellent softness, however, the hydrophilicity of the treated cotton fabric is reduced. It is necessary to modify Amino-silicone oil with polyether in order to improve the hydrophilicity of the treated fabric. However, the existing product is difficult to give consideration to the softness and hydrophilicity at the same time. Therefore, in this paper, the three kinds of hydrophilic silicone softener finishing agents—the amio-silicone modified with epoxy group polyether, the polydimethylsiloxane-polyether block copolymers terminated quaternary ammonium salt and the novel linear silicone aminopolyalkyleneoxide block copolymer modified by quaternary ammonium salt had been synthesized, and their application property had been also discussed to afford some information in the synthesis of a new better performance hydrophilic silicone softener finishing agent. The contents and results of researchs are as follows:Part one: Study on preparation and application property of amio-silicone modified with epoxy group polyether. Self-emulsifying amino-silicone modified with epoxy group polyether (PMAS) were prepared with epoxy group polyether and amino-silicone (AS) as the raw material in the presence of isopropyl alcohol. The effect of these factors such as the amino value and the viscosity of AS, and the mole ratio of amino of amino-silicone to the epoxy group of polyether on the particle size of PMAS emulsion and the softness,hydrophilicity and whiteness of fabric finished with PMAS, the conditions of the reaction were optimized. The influence of finishing technology factors such as dosage of PMAS, baking temperature and baking time on the properties of the cotton fabric finished with PMAS were investigated, the finishing technology conditions of PMAS were optimized, and the application properties of the cotton fabric finished with PMAS were tested, and compared with that of AS and similar modified amino-silicone in market. The results indicated that when the amino value and viscosity of AS were 0.9mmol/g and 1450mPa·s, and the mole ratio of the amino of amino-silicone to epoxy group of polyether was 1:1, the synthetic PMAS could self–emulsify, its emulsion possesses good stability, and the optimal pad finishing process of PMAS are as follows: the dosage of PMAS was 10g/L, the baking temperature and baking time was 140℃×50s. The cotton fabric finished with PMAS possessed as good soft as and much better hydrophilic than that of the fabric treated with AS. However, Compared with similar modified amino-silicone in market, the hydrophilicity of AS modified by epoxy group polyether should be improved further.Part two: Study on preparation and application property of polydimethylsiloxane-polyether block copolymers terminated quaternary ammonium salt.The linear polydimethylsiloxane-polyether block copolymers terminated by quaternary ammonium salt (QASTSP) had been synthesized. Firstly, polydimethylsiloxane -polyether block copolymersterminated epoxy group (ETSP) were prepared with allyl glycidyl ether (AGE) and polydimethylsiloxane-polyether block copolymers terminated by dihydrogen(HTSP) which was prepared with polysiloxanes terminated byα,ω-dihydrogen and polyether terminated byα,ω-allyl (ATP) as the raw materials in the solvent of ethyl acetate. Then QASTSP was obtained by the quaternization between ETSP and octadecyl dimethyl tertiary amine with isopropanol as solvent. The effect of these factors such as the molar ratio of HTSP to ATP, reaction temperature, the reaction time, and the amounts of solvent on the synthesis of the intermediate product——HTSP and the synthesis of the target compound——QASTSP were investigated, the conditions of the reaction were optimized. The structure of the ETSP was determined by FTIR,1HNMR. Finally,these factors such as dosage of QASTSP, baking temperature and baking time, which affect the hydrophilicity and softness of QASTSP were studied, the conditions of pad finishing process of QASTSP were optimized, and the application properties of the cotton fabric finished with QASTSP were tested, and compared with that of AS and similar modified amino-silicone product in market. The results indicated that the optimum conditions of the synthesis of HTSP were that the molar ratio of HTSP to ATP was 1.2:1, the reaction temperature was 75℃, the reaction time was 3h, the catalyst mass content was 0.10%, the amounts of dissolvent was 35%wt.The optimal reaction conditions of the synthesis of QASTSP were that the reaction temperature was 90℃, the reaction time was 4.5h, the amount of dissolvent was 30%wt.The optimum pad finishing process of QASTSP were as follows: dosage of QASTSP was 8g/L, baking temperature and baking time was 140℃×30s. The cotton fabric finished with QASTSP possessed good softness and hydrophilicity. However, compared with amino-silicone softener, the softness and the washing fastness of QASTSP should be improved further.Part three: Study on preparation and application property of novel linear silicone aminopolyalkyleneoxide block copolymer modified by quaternary ammonium salt. A novel linear silicone aminopolyalkyleneoxide block copolymer modified by quaternary ammonium salt (QAPAMS) was synthesized by three steps. Firstly, epoxy-terminated polydimethylsiloxane (ETPS) was prepared with polydimethylsioxane terminated by hydrogen and allyl glycidyl ether as the raw materials by hydrosilication reaction. Secondly, silicone aminopolyalkyleneoxide block copolymer (SAPB) was synthesized with epoxy-terminated polydimethylsiloxane (ETPS) and polyether terminated by aminopropyl (ED-600) at the present of some solvent. Thirdly, a novel linear silicone aminopolyalkyleneoxide block copolymer modified by quaternary ammonium salt (QAPAMS) was synthesized with glycidtrimethylammonium chloride (EPTAC) and silicone aminopolyalkyleneoxide block copolymer. The effect of these factors of SAPB on its viscosity such as the molar ratio of ETPS to ED-600, reaction temperature, the reaction time, and the amounts of solvent were researched, the synthesis technology factors of novel linear silicone aminopolyalkyleneoxide block copolymers modified by quaternary ammonium salt (QAPAMS) on the conversion were also investigated, and the conditions of these reactions were optimized. The structure of ETPS and SAPB were determined by FTIR,1HNMR,GPC. The influence of these factors such as dosage of finishing, baking temperature and baking time on the application property of QAPAMS were studied, the conditions of finishing process of QAPAMS were optimized, and the application properties of the cotton fabric finished with QAPAMS were tested, and compared with that of AS and other hydrophilic modified amino-silicone. The results indicated that the conditions of the synthesis of SAPB were that the molar ratio was 1.2:1 (ETPS/ED-600), the reaction temperature was 80℃,the reaction time was 5h, and the dissolvent was 30%wt. The optimum conditions of the synthesis of QAPAMS were that the molar ratio of amino of SAPB to the epoxy group of EPTAC was 1:1.1, the reaction temperature was 70℃,the reaction time was 5h,and the dissolvent was15%wt. The optimum conditions of pad finishing process of QAPAMS were that dosage of finishing agent was 6g/L, baking temperature and baking time was 140℃×50s, the softness, hydrophilicity and washing fastness of the fabric treated with QAPAMS was desirable, compared with that of AS, PMAS, QASTSP, and similar hydrophilic modified amino-silicone product in market.Compared with the application property of AS, PMAS, QASTSP, and similar hydrophilic modified amino-silicone product in market, the cotton fabric finished with PMAS possessed as good soft as and much better hydrophilic than that of the fabric treated with AS. However, the hydrophilicity of AS modified by epoxy group polyether was still poor. The cotton fabric finished with QASTSP possessed good softness and hydrophilicity. However, compared with amino-silicone softener, the washing fastness of QASTSP was poor. The fabric treated with QAPAMS possessed good softness, hydrophilicity and washing fastness, and match to that of similar hydrophilic modified amino-silicone product in market. The results show that the modified method of QAPAMS for silicone softener is fine to synthesize hydrophilic silicone softener. |
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