CN103087326A - Preparation method of polyoxy alkyl epoxy modified amino silicon oil softening agent - Google Patents
Preparation method of polyoxy alkyl epoxy modified amino silicon oil softening agent Download PDFInfo
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- CN103087326A CN103087326A CN2012105965844A CN201210596584A CN103087326A CN 103087326 A CN103087326 A CN 103087326A CN 2012105965844 A CN2012105965844 A CN 2012105965844A CN 201210596584 A CN201210596584 A CN 201210596584A CN 103087326 A CN103087326 A CN 103087326A
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Abstract
The invention discloses a preparation method of a polyoxy alkyl epoxy modified amino silicon oil softening agent. The preparation method of the polyoxy alkyl epoxy modified amino silicon oil softening agent comprises a formula and a preparation method. According to the invention, a copolymer of an amino silane coupling agent and octamethylcyclotetrasiloxane is modified, and an epoxy group of active polyoxy alkyl epoxy group ether is grafted on a side chain of amino silane so as to obtain the polyoxy alkyl epoxy modified amino silicon oil softening agent; and therefore, the yellowing, the moisture adsorption permeability and fluffy sense of tided fabrics are improved; the reaction activity, the compatibility and the easily emulsifying performance of the softening agent are improved; and the defects of serious yellowing, poor moisture adsorption permeability and poor fluffy sense in the prior art are overcome. The fabrics are tidied by using the prepared softening agent, so that the tided fabrics fulfill the aims of reducing the yellowing and improving the moisture adsorption permeability and the fluffy sense.
Description
Technical field
The present invention relates to a kind of preparation method of fabric softener.Specifically refer to the preparation method for a kind of polyoxy alkyl epoxy modified amino-silicone oil softening agent that textile fabric is carried out the soft fluffy arrangement.
Background technology
Yarn fabric is in rear arrangement process, needing to use softening agent to carry out soft fluffy to fabric processes, with sense of touch and the impression of improving fabric, prior art adopts amido silicon oil as softening agent, fabric to be carried out soft fluffy and arranges, serious due to the fabric xanthochromia that amino-silicone oil softening agent arranges, sucting wet air permeability is poor, fluffy sense is not good enough, therefore, there are the problems and shortcomings that xanthochromia is serious, sucting wet air permeability is poor, fluffy sense is not good enough in prior art.
Summary of the invention
problems and shortcomings for above-mentioned prior art existence, the present invention adopts the multipolymer to amino silicane coupling agent and octamethylcyclotetrasiloxane to carry out modification, the epoxide group of the active polyoxy alkyl epoxy of grafting base ether on the side chain of aminosilane, obtain a kind of softening agent of polyoxy alkyl epoxy modified amino silicon oil, be organized the xanthochromia of fabric with improvement, sucting wet air permeability and fluffy sense, to improve the reactive behavior of softening agent, the technical scheme of consistency and easy emulsifying property, a kind of preparation method of polyoxy alkyl epoxy modified amino-silicone oil softening agent is provided, be intended to prepared softening agent finish fabric, make and be organized fabric and reach the minimizing xanthochromia, improve the purpose of sucting wet air permeability and fluffy sense.
The object of the present invention is achieved like this: a kind of preparation method of polyoxy alkyl epoxy modified amino-silicone oil softening agent, comprise formula and preparation method, wherein:
Described formula is,
A silane coupling agent: N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 1.8%;
B silane coupling agent: γ-diethylenetriamine propyl group methyl dimethoxysilane, 0.9%;
Hydrolytic reagent: deionized water, 0.63%;
Basic monomer: octamethylcyclotetrasiloxane, 81.9%;
Modified monomer: butyl polyoxyethylene polyoxypropylene epoxy group(ing) ether, 4.7%;
Closure agent: hexamethyldisiloxane, 0.62%;
Catalyzer: potassium hydroxide, 0.05%;
Solvent: propyl carbinol, 9.4%;
The formula unit is mass percent;
Described preparation method is polymerization,
The preparation of step 1, hydrolyzation material
A silane coupling agent, B silane coupling agent and hydrolytic reagent in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 90 ℃, insulation reaction, fully is hydrolyzed the A/B coupling agent at 2 hours insulation reaction used times, then be cooled to 40 ℃, vacuum is pulled out low-boiling-point substance under 0.095 atmospheric vacuum condition, and vacuum is pulled out 20 minutes used times, makes the hydrolyzation material that contains the A/B coupling agent;
The copolymerization of step 2, hydrolyzation material and basic monomer
basic monomer and described hydrolyzation material in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 95 ℃, heated and stirred 20 minutes, add afterwards the closure agent in formula, reactor is warming up to 120 ℃, continued heated and stirred 20 minutes, add again afterwards the catalyzer in formula, continue to stir, open simultaneously nitrogen and fill nitrogen in reactor, and the opening pressure equilibrium valve makes nitrogen atmosphere pressure and external atmosphere pressure maintenance running balance in reactor, it is 5～8 bubbles per second clocks of reducing valve that the interior nitrogen of reactor outwards overflows speed, afterwards, reactor is warming up to 140 ℃, carry out copolyreaction under this temperature and nitrogen atmosphere, 1 hour used time of reaction, close afterwards nitrogen, continued insulation reaction 3～4 hours, reactor cools to room temperature afterwards, make the copolymerization amido silicon oil.
Step 3, modified monomer carry out the epoxide polymerization modification to the copolymerization amido silicon oil
with the modified monomer in formula, solvent and described copolymerization amido silicon oil join in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 80 ℃ and is incubated polyreaction, after reaction solution bleach in the question response still, continued again insulation reaction 4 hours, reactor is cooled to 40 ℃ afterwards, open vacuum valve to reaction kettle for vacuumizing, vacuum tightness is 0.095 normal atmosphere, vacuum is pulled out the solvent in reaction solution in still, vacuum is pulled out 20 minutes used times, reactor cools to room temperature afterwards, obtain polyoxy alkyl epoxy modified amino silicon oil goods.
The easy emulsification of goods of the present invention and emulsion-stabilizing performance are good, and the fabric that arranges can not only obtain softness, smooth plentiful feel, and xanthochromia is little; Owing to not containing the non-environmental protection components such as formaldehyde, phenyl ring in formula of the present invention, the solvent that adopts can recycling, has both reduced cost, also be conducive to environment protection, so goods of the present invention is the environment-friendly type goods.
above-mentioned, the present invention adopts the multipolymer to amino silicane coupling agent and octamethylcyclotetrasiloxane to carry out modification, the epoxide group of the active polyoxy alkyl epoxy of grafting base ether on the side chain of aminosilane, obtain a kind of softening agent of polyoxy alkyl epoxy modified amino silicon oil, be organized the xanthochromia of fabric with improvement, sucting wet air permeability and fluffy sense, to improve the reactive behavior of softening agent, the technical scheme of consistency and easy emulsifying property, having overcome prior art exists xanthochromia serious, sucting wet air permeability is poor, the problems and shortcomings that fluffy sense is not good enough, the preparation method of a kind of polyoxy alkyl epoxy modified amino-silicone oil softening agent that provides, with prepared softening agent finish fabric, make and be organized fabric and reached the minimizing xanthochromia, improve the purpose of sucting wet air permeability and fluffy sense.
The embodiment explanation
Below by the preparation method of specific embodiment to a kind of polyoxy alkyl epoxy modified amino-silicone oil softening agent of the present invention, be described in further detail, the those skilled in the art can make polyoxy alkyl epoxy modified amino-silicone oil softening agent with reference to formula and the preparation method of embodiment, but should not be construed as any limitation of the invention.
Embodiment
Embodiment
The name of an article: polyoxy alkyl epoxy modified amino-silicone oil softening agent
Formula: the unit of filling a prescription is weight percentage;
A silane coupling agent: N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 1.8%;
B silane coupling agent: γ-diethylenetriamine propyl group methyl dimethoxysilane, 0.9%;
Hydrolytic reagent: deionized water, 0.63%;
Basic monomer: octamethylcyclotetrasiloxane, 81.9%;
Modified monomer: butyl polyoxyethylene polyoxypropylene epoxy group(ing) ether, 4.7%;
Closure agent: hexamethyldisiloxane, 0.62%;
Catalyzer: potassium hydroxide, 0.05%;
Solvent: propyl carbinol, 9.4%;
Preparation
Preparation condition, equipment
Ambient pressure a: normal atmosphere;
Envrionment temperature: room temperature;
Preparation equipment and supporting: reactor, supporting with source nitrogen and vacuum source.
The preparation method is polymerization,
The preparation of step 1, hydrolyzation material
A silane coupling agent, B silane coupling agent and hydrolytic reagent in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 90 ℃, insulation reaction, fully is hydrolyzed the A/B coupling agent at 2 hours insulation reaction used times, then be cooled to 40 ℃, vacuum is pulled out low-boiling-point substance under 0.095 atmospheric vacuum condition, and vacuum is pulled out 20 minutes used times, makes the hydrolyzation material that contains the A/B coupling agent;
The copolymerization of step 2, hydrolyzation material and basic monomer
basic monomer and described hydrolyzation material in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 95 ℃, heated and stirred 20 minutes, add afterwards the closure agent in formula, reactor is warming up to 120 ℃, continued heated and stirred 20 minutes, add again afterwards the catalyzer in formula, continue to stir, open simultaneously nitrogen and fill nitrogen in reactor, and the opening pressure equilibrium valve makes nitrogen atmosphere pressure and external atmosphere pressure maintenance running balance in reactor, it is 5～8 bubbles per second clocks of reducing valve that the interior nitrogen of reactor outwards overflows speed, afterwards, reactor is warming up to 140 ℃, carry out copolyreaction under this temperature and nitrogen atmosphere, 1 hour used time of reaction, close afterwards nitrogen, continued insulation reaction 3～4 hours, reactor cools to room temperature afterwards, make the copolymerization amido silicon oil.
Step 3, modified monomer carry out the epoxide polymerization modification to the copolymerization amido silicon oil
with the modified monomer in formula, solvent and described copolymerization amido silicon oil join in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 80 ℃ and is incubated polyreaction, after reaction solution bleach in the question response still, continued again insulation reaction 4 hours, reactor is cooled to 40 ℃ afterwards, open vacuum valve to reaction kettle for vacuumizing, vacuum tightness is 0.095 normal atmosphere, vacuum is pulled out the solvent in reaction solution in still, vacuum is pulled out 20 minutes used times, reactor cools to room temperature afterwards, obtain polyoxy alkyl epoxy modified amino silicon oil goods.
Purposes, usage and the storage of the polyoxy alkyl epoxy modified amino silicon oil goods that the present invention makes:
Purposes: the soft fluffy that is used for fabric arranges;
Usage: with padding or soaking technology is processed fabric;
Store: antifreeze, the lucifuge sealing is preserved.
Claims (1)
1. the preparation method of a polyoxy alkyl epoxy modified amino-silicone oil softening agent, comprise formula and preparation method, it is characterized in that:
Described formula is,
A silane coupling agent: N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane, 1.8%;
B silane coupling agent: γ-diethylenetriamine propyl group methyl dimethoxysilane, 0.9%;
Hydrolytic reagent: deionized water, 0.63%;
Basic monomer: octamethylcyclotetrasiloxane, 81.9%;
Modified monomer: butyl polyoxyethylene polyoxypropylene epoxy group(ing) ether, 4.7%;
Closure agent: hexamethyldisiloxane, 0.62%;
Catalyzer: potassium hydroxide, 0.05%;
Solvent: propyl carbinol, 9.4%;
The formula unit is mass percent;
Described preparation method is polymerization,
The preparation of step 1, hydrolyzation material
A silane coupling agent, B silane coupling agent and hydrolytic reagent in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 90 ℃, insulation reaction, fully is hydrolyzed the A/B coupling agent at 2 hours insulation reaction used times, then be cooled to 40 ℃, vacuum is pulled out low-boiling-point substance under 0.095 atmospheric vacuum condition, and vacuum is pulled out 20 minutes used times, makes the hydrolyzation material that contains the A/B coupling agent;
The copolymerization of step 2, hydrolyzation material and basic monomer
basic monomer and described hydrolyzation material in formula are joined stirring heating in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 95 ℃, heated and stirred 20 minutes, add afterwards the closure agent in formula, reactor is warming up to 120 ℃, continued heated and stirred 20 minutes, add again afterwards the catalyzer in formula, continue to stir, open simultaneously nitrogen and fill nitrogen in reactor, and the opening pressure equilibrium valve makes nitrogen atmosphere pressure and external atmosphere pressure maintenance running balance in reactor, it is 5～8 bubbles per second clocks of reducing valve that the interior nitrogen of reactor outwards overflows speed, afterwards, reactor is warming up to 140 ℃, carry out copolyreaction under this temperature and nitrogen atmosphere, 1 hour used time of reaction, close afterwards nitrogen, continued insulation reaction 3～4 hours, reactor cools to room temperature afterwards, make the copolymerization amido silicon oil.
Step 3, modified monomer carry out the epoxide polymerization modification to the copolymerization amido silicon oil
with the modified monomer in formula, solvent and described copolymerization amido silicon oil join in reactor, agitator speed is 200～300 rev/mins, reactor is warming up to 80 ℃ and is incubated polyreaction, after reaction solution bleach in the question response still, continued again insulation reaction 4 hours, reactor is cooled to 40 ℃ afterwards, open vacuum valve to reaction kettle for vacuumizing, vacuum tightness is 0.095 normal atmosphere, vacuum is pulled out the solvent in reaction solution in still, vacuum is pulled out 20 minutes used times, reactor cools to room temperature afterwards, obtain polyoxy alkyl epoxy modified amino silicon oil goods.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835716A (en) * | 2017-02-28 | 2017-06-13 | 青岛奥洛思新材料有限公司 | For processing wool or smooth brightening agent containing wool fabric and preparation method thereof |
| CN107936256A (en) * | 2017-11-20 | 2018-04-20 | 杭州美高华颐化工有限公司 | A kind of preparation method of modified side chain block silicone oil |
| CN113957721A (en) * | 2021-10-27 | 2022-01-21 | 浙江汉邦新材料股份有限公司 | Crease-resistant elastic silicone oil and preparation method thereof |
| CN114197214A (en) * | 2021-12-28 | 2022-03-18 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarn and preparation method thereof |
Citations (1)
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|---|---|---|---|---|
| CN1657687A (en) * | 2005-01-17 | 2005-08-24 | 中山市巴斯基化工有限公司 | Hydrophilic ammonia hydrocarbon base polystoxane softening agent and its preparation method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657687A (en) * | 2005-01-17 | 2005-08-24 | 中山市巴斯基化工有限公司 | Hydrophilic ammonia hydrocarbon base polystoxane softening agent and its preparation method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835716A (en) * | 2017-02-28 | 2017-06-13 | 青岛奥洛思新材料有限公司 | For processing wool or smooth brightening agent containing wool fabric and preparation method thereof |
| CN106835716B (en) * | 2017-02-28 | 2019-01-01 | 青岛奥洛思新材料有限公司 | For handling wool or the smooth brightening agent containing wool fabric and preparation method thereof |
| CN107936256A (en) * | 2017-11-20 | 2018-04-20 | 杭州美高华颐化工有限公司 | A kind of preparation method of modified side chain block silicone oil |
| CN107936256B (en) * | 2017-11-20 | 2020-07-17 | 杭州美高华颐化工有限公司 | Preparation method of side chain modified block silicone oil |
| CN113957721A (en) * | 2021-10-27 | 2022-01-21 | 浙江汉邦新材料股份有限公司 | Crease-resistant elastic silicone oil and preparation method thereof |
| CN113957721B (en) * | 2021-10-27 | 2023-09-29 | 浙江汉邦新材料股份有限公司 | Anti-wrinkle elastic silicone oil and preparation method thereof |
| CN114197214A (en) * | 2021-12-28 | 2022-03-18 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarn and preparation method thereof |
| CN114197214B (en) * | 2021-12-28 | 2024-03-29 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarns and preparation method thereof |
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