CN101509196A - Method of preparing epoxy modified amino-silicone oil softening agent - Google Patents
Method of preparing epoxy modified amino-silicone oil softening agent Download PDFInfo
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Abstract
The invention discloses a method for preparing epoxy modified amino silicon oil softening agent, which comprises the following steps: mixing amino silane coupling agent and polysiloxane monomer in an alkali catalyst at a temperature of between 70 and 80 DEG C; reacting the amino silane coupling agent and the polysiloxane monomer at a temperature of between 90 and 150 DEG C to generate amino silicon oil and low-boiling-point substances; distilling the low-boiling-point substances; reducing the temperature to between 40 and 80 DEG C to obtain the amino silicon oil; reacting the amino silicon oil and epoxy chloropropane in an inert solvent for 1 to 5 hours at a temperature of between 40 and 120 DEG C to generate epoxy modified amino silicon oil; removing the inert solvent to obtain the epoxy modified amino silicon oil; and adding the epoxy modified amino silicon oil into an emulsifying agent to emulsify, and adjusting the pH value to be 6 to 7 to obtain the epoxy modified amino silicon oil softening agent. The method reacts the amino silicon oil and the epoxy chloropropane in the inert solvent to obtain the epoxy modified amino silicon oil; and because the amino is increased with an epoxy group to active hydrogen on the amino, the epoxy modified amino silicon oil softening agent has better stability, softness and neatness.
Description
Technical field
The present invention relates to a kind of preparation method of softener, relate in particular to a kind of preparation method of epoxy modified amino-silicone oil softening agent.
Background technology
Amido silicon oil has good submissive and bating effect because of it to fabric, and therefore, amino silicon oil emulsion is commonly used to as fabric softener.After but many synthetic fabrics such as terylene, polyester cotton blending etc. were put in order through common amino silicon oil emulsion, feel was greasy, lacks the style of natural lining, and very degree of scraping is also not enough, simultaneously because oxidation makes the easy flavescence of lining.
Therefore, prior art awaits to improve and development.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of epoxy modified amino-silicone oil fabric softener, the fabric softener of the method preparation overcomes the technological deficiency that existing on the market fabric softener exists, and promptly utilizes this method to prepare to have the improved flexibility and the fabric softener of degree of scraping very.
Technical scheme of the present invention is as follows:
A kind of preparation method of epoxy modified amino-silicone oil softening agent, this method may further comprise the steps:
A, with amino silicane coupling agent and silicone monomers complete miscibility under the temperature conditions of base catalyst and 70-80 ℃;
B, elevated temperature also are controlled in the 90-150 ℃ of scope, and described amino silicane coupling agent and silicone monomers are reacted in this temperature range, generate amido silicon oil and low-boiling-point substance;
C, vacuumize and distillate low-boiling-point substance;
D, reduce temperature and be controlled at 40-80 ℃ of scope, separate obtaining amido silicon oil;
E, amido silicon oil was reacted 1-5 hour under 40-120 ℃ temperature conditions with epoxychloropropane in atent solvent, generate epoxy modified amino-silicone oil;
F, removal atent solvent obtain epoxy modified amino-silicone oil;
G, epoxy modified amino-silicone oil added carry out emulsification in the emulsifying agent, and adopt weak acid that the pH value of emulsion is adjusted to 6-7, then obtain epoxy modified amino-silicone oil softening agent.
Described preparation method, wherein, described step C specifically comprises step:
C1, under 90-150 ℃ temperature conditions, be evacuated to 0.02-0.03mpa, distillate low-boiling-point substance;
C2, gas clean-up reach in the scope of 1000-20000cs its material viscosity to 0.05-0.1mpa, and low-boiling-point substance distillates fully, stops to vacuumize.
Described preparation method, wherein, described step F specifically may further comprise the steps:
F1, under the vacuum condition of 60-100 ℃ temperature and 0.03-0.06mpa, remove atent solvent.
Described preparation method, wherein, described amino silicane coupling agent is one or more of following component: N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl methyldiethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane, N-cyclohexyl-y-aminopropyl methyl dimethoxysilane, γ-piperazinyl propyl group methyl dimethoxysilane.
Described preparation method, wherein, described silicone monomers is one or more of following component: octamethylcy-clotetrasiloxane, methyl cyclosiloxane mix monomer, the linear hydroxy-end capped silicone oil of low molecular weight.
Described preparation method, wherein, described base catalyst is a TMAH.
Described preparation method, wherein, described atent solvent is toluene or dimethylbenzene.
Described preparation method, wherein, described emulsifying agent is one or more of following component: alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, isomery fatty alcohol-polyoxyethylene ether.
Described preparation method, wherein, described amino silicane coupling agent and silicone monomers mass ratio are between the 1:199-1:9.
Described preparation method, wherein, the quality of described base catalyst accounts for the 0.3%-1% of described amino silicane coupling agent and silicone monomers quality summation.
Described preparation method, wherein, described epoxychloropropane and amino silicane coupling agent mol ratio are between 3:10-1:1.
Described preparation method, wherein, the mass ratio of described atent solvent and amido silicon oil is 1:10-1:1.
Described preparation method, wherein, the mass ratio of described emulsifying agent and epoxy modified amino-silicone oil is 0.3-0.5.
Described preparation method, wherein, the described weak acid among the described step G is acetic acid.
The preparation method of a kind of epoxy modified amino-silicone oil softening agent provided by the present invention, its method with amido silicon oil in atent solvent with epichlorohydrin reaction, obtain epoxy modified amino-silicone oil, owing to reduced the active hydrogen on the amino having increased epoxide group on the amino, it is compared with common amido silicon oil in the prior art, stability is high, and be applied the flexibility, slippery of fabric, very scrape Du Genggao, and little to the influence of lining whiteness.
Description of drawings
Fig. 1 is various embodiments of the present invention and raw material, process conditions and product property index mapping relations table;
Fig. 2 is the continuous table of Fig. 1;
Fig. 3 is the continuous table of Fig. 2.
The specific embodiment
The operating procedure of various embodiments of the present invention is basic identical, but the raw material that each embodiment adopted, with and consumption be not quite similar, the process conditions that adopted simultaneously are difference to some extent also, therefore, the performance indications of its end product also have fine distinction, various embodiments of the present invention and raw material, process conditions and product property index mapping relations are as Fig. 1, Fig. 2, shown in Figure 3.
Each performance indications aspect of raw material, raw material consumption, process conditions, operating procedure and final products from being adopted is described in detail each preferred embodiment of the present invention below.
The preparation process of epoxy modified amino-silicone oil softening agent is as follows: get 6 gram N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilanes and 194 gram methyl cyclosiloxane mix monomer DMC mix, and adding 0.6g TMAH base catalyst, stir and heat up, and control temperature T 1 is 70 ℃;
Observe and to judge whether complete miscibility of described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and methyl cyclosiloxane mix monomer DMC, after treating complete miscibility, continue to heat up, and control T2 is 90 ℃, at this moment, described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and methyl cyclosiloxane mix monomer DMC react, and generate amido silicon oil and low-boiling-point substance;
Vacuumizing and making its vacuum 1 is 0.025mpa, distillates low-boiling-point substance; Gas clean-up 2 is to 0.075mpa, and when material viscosity 1 reached 1000cs, at this moment, described low-boiling-point substance was considered as distillating fully, then stop pumping vacuum;
Lowering the temperature and making its control T3 is 50 ℃, obtains amido silicon oil; Amido silicon oil is in time added in the 100ml dimethylbenzene atent solvent, agitation and dilution, and then add the 2.7g epoxychloropropane, and be reaction 1 hour under 60 ℃ the temperature conditions at T4 with it;
Control intensification T5 is 70 ℃ and control vacuum 3 for removing dimethylbenzene atent solvent (can recycling use) under the condition of 0.05mpa, obtains epoxy modified amino-silicone oil;
Calculate by weight and take by weighing 2 parts of epoxy modified amino-silicone oils, 1 part of alkylphenol polyoxyethylene (EO several 4～10), and adopt micro-emulsion technology to make the blue light transparent micro emulsion, adjusting described ph value of emulsion by HAC at last, to make the pH value be 7, promptly obtains the epoxy modified amino-silicone oil fabric softener.Discover that after tested the fabric panel slippery of handling through this softener better, very degree of scraping is higher, less to the influence of lining whiteness simultaneously, stability is high.
The preparation process of the epoxy modified amino-silicone oil softening agent of present embodiment is as follows: get 10 gram γ-divinyl triammonium propyl group methyl dimethoxysilanes and 190 gram octamethylcy-clotetrasiloxane D
4Mix, and add 1.3g TMAH base catalyst, stir and heat up, control temperature T 1 is 72 ℃;
Observe and judge described γ-divinyl triammonium propyl group methyl dimethoxysilane and octamethylcy-clotetrasiloxane D
4Complete miscibility whether, treat complete miscibility after, continue to heat up, and control T2 is 140 ℃, at this moment, described γ-divinyl triammonium propyl group methyl dimethoxysilane and octamethylcy-clotetrasiloxane D
4React, generate amido silicon oil and low-boiling-point substance;
Vacuumizing and making its vacuum 1 is 0.03mpa, distillates low-boiling-point substance; Slowly gas clean-up 2 is to 0.1mpa again, and when material viscosity 1 reached 5000cs, at this moment, described low-boiling-point substance was considered as distillating fully, then stop pumping vacuum;
Lower the temperature T3 to 40 ℃, obtain amido silicon oil; Amido silicon oil in time being added in the 120ml toluene atent solvent, behind the agitation and dilution, add the 3.7g epoxychloropropane, is reaction 2 hours under 40 ℃ the temperature conditions at T4;
Elevated temperature and to control temperature T 5 be 90 ℃ and control vacuum 3 for removing toluene atent solvent (can recycling use) under the condition of 0.06mpa obtains epoxy modified amino-silicone oil;
Calculating takes by weighing 3 parts of epoxy modified amino-silicone oils by weight, 2 parts of fatty alcohol-polyoxyethylene ether (EO several 3～10) are mixed, and adopt micro-emulsion technology to make the blue light transparent micro emulsion, pH value with HAC adjustment emulsion is 6 at last, promptly obtains epoxy modified amino-silicone oil softening agent.Discover after tested,, very degree of scraping height fine through the fabric panel slippery that this softener was handled, little to the influence of lining whiteness simultaneously, stability is very high.
The preparation method of present embodiment epoxy modified amino-silicone oil softening agent is as follows: get 12 gram γ-piperazinyl propyl group methyl dimethoxysilanes and the linear hydroxy-end capped silicone oil of 188 gram low molecular weights mixes, and adding 2.0g TMAH base catalyst, stir and heat up, and control temperature T 1 is 74 ℃;
Observe and to judge whether complete miscibility of described γ-piperazinyl propyl group methyl dimethoxysilane and the hydroxy-end capped silicone oil of low molecular weight linearity, after treating complete miscibility, continue to heat up, and to control its temperature T 2 be 120 ℃, at this moment, the linear hydroxy-end capped silicone oil of described γ-piperazinyl propyl group methyl dimethoxysilane and low molecular weight reacts, and generates amido silicon oil and low-boiling-point substance;
Vacuumizing and making its vacuum 1 is 0.02mpa, distillates low-boiling-point substance; Slowly gas clean-up 2 is to 0.05mpa again, and when material viscosity 1 reached 10000cs, at this moment, described low-boiling-point substance was considered as distillating fully, then stop pumping vacuum, and cooling T3 is 80 ℃, obtains amido silicon oil;
Amido silicon oil is in time added in the 60ml toluene atent solvent, and agitation and dilution adds the 2.4g epoxychloropropane again, is reaction 3 hours under 120 ℃ the condition in temperature T 4;
In temperature T 5 is 80 ℃, vacuum 3 for removing toluene atent solvent (can recycle and reuse) under the condition of 0.03mpa, obtains epoxy modified amino-silicone oil;
Take by weighing 7 parts of epoxy modified amino-silicone oils, 3 parts of isomery fatty alcohol-polyoxyethylene ether (EO several 5～10) by weight calculating, and adopt micro-emulsion technology to make the blue light transparent micro emulsion, making its pH value with HAC adjustment ph value of emulsion at last is 6.5, promptly obtains epoxy modified amino-silicone oil softening agent.Discover that after tested the fabric panel slippery of handling through this softener is good, very degree of scraping is very high, very little to the influence of lining whiteness simultaneously, stability is high.
The preparation method of present embodiment epoxy modified amino-silicone oil softening agent, its detailed process is as follows: get 1 gram N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and 199 gram octamethylcy-clotetrasiloxane D
4Mix, and add 1.0g TMAH base catalyst, stir and heat up, and control temperature T 1 is 76 ℃;
Observe and judge described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and octamethylcy-clotetrasiloxane D
4Complete miscibility whether, treat complete miscibility after, continuing to be warming up to T2 is 100 ℃, at this moment, described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and octamethylcy-clotetrasiloxane D
4React, generate amido silicon oil and low-boiling-point substance;
Vacuumizing and making its vacuum 1 is 0.023mpa, distillates low-boiling-point substance; Slowly gas clean-up 2 is to 0.09mpa again, and when material viscosity 1 reached 15000cs, at this moment, described low-boiling-point substance was considered as distillating fully, then stop pumping vacuum, and lowering the temperature and making its control T3 is 60 ℃, obtains amido silicon oil;
Amido silicon oil is in time added in the 80ml toluene atent solvent, and agitation and dilution, and then add the 0.27g epoxychloropropane is reaction 4 hours under 80 ℃ the temperature conditions at T4; Control temperature T 5 is that 100 ℃ and vacuum 3 remove toluene atent solvent (can recycling use) under the condition of 0.04mpa, obtains epoxy modified amino-silicone oil;
Take by weighing 5.5 parts of epoxy modified amino-silicone oils, 4.5 parts of alkylphenol polyoxyethylene (EO several 4～10) by weight calculating, and adopt micro-emulsion technology to make the blue light transparent micro emulsion, adjusting ph value of emulsion with HAC at last is 7, promptly obtain the epoxy modified amino-silicone oil fabric softener, discover after tested,, very degree of scraping height fine through the fabric panel slippery that this softener was handled, little to the influence of lining whiteness simultaneously, stability is high.
The preparation process of present embodiment epoxy modified amino-silicone oil softening agent is as follows: get 20 gram N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilanes and the linear hydroxy-end capped silicone oil of 180 gram low molecular weights mixes, and adding 1.7g TMAH base catalyst, stir and heat up, and control temperature T 1 is 80 ℃;
Observe and to judge whether complete miscibility of described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and the hydroxy-end capped silicone oil of low molecular weight linearity, after treating complete miscibility, continue to heat up, and control T2 is 150 ℃, at this moment, the linear hydroxy-end capped silicone oil of described N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane and low molecular weight reacts, and generates amido silicon oil and other low-boiling-point substances;
Vacuumizing and making its vacuum 1 is about 0.03mpa, distillates low-boiling-point substance; Slowly gas clean-up 2 is to 0.05mpa again, and when material viscosity 1 reached 20000cs, at this moment, described low-boiling-point substance was considered as distillating fully, then stop pumping vacuum, and lowering the temperature and making its control T3 is 65 ℃, obtains amido silicon oil;
Amido silicon oil is in time added in the 130ml dimethylbenzene atent solvent, and agitation and dilution adds the 2.7g epoxychloropropane again, is reaction 5 hours under 100 ℃ the temperature conditions at T4; The control temperature removes dimethylbenzene atent solvent (can recycle and reuse) under T5 is 60 ℃ and the condition of vacuum 3 at 0.045mpa, obtain epoxy modified amino-silicone oil;
Take by weighing 6.5 parts of epoxy modified amino-silicone oils, 3.5 parts of fatty alcohol-polyoxyethylene ether (EO several 3～10) by weight calculating, and adopt micro-emulsion technology to make the blue light transparent micro emulsion, making its pH value with HAC adjustment ph value of emulsion at last is 7, promptly obtains epoxy modified amino-silicone oil softening agent.Discover after tested, the fabric panel slippery of handling through this softener better, degree of scraping height very, less to the influence of lining whiteness simultaneously, stability is high.
The epoxy modified amino-silicone oil softening agent that the method that the invention provides is prepared, owing to reduced the active hydrogen on the amino having increased epoxide group on the amino, and adopt specific process conditions in the preparation process, it is compared with common amino-silicone oil softening agent in the prior art, stability is high, be applied fabric flexibility, slippery, very degree of scraping is better, and is and little to lining whiteness influence.
Should be understood that the present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, the above embodiment of the present invention can only be thought can not limit the present invention to explanation of the present invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore in implication suitable and any change in the scope, all should think to be included in the scope of claims with claims of the present invention.
Claims (14)
1, a kind of preparation method of epoxy modified amino-silicone oil softening agent, this method may further comprise the steps:
A, with amino silicane coupling agent and silicone monomers complete miscibility under the temperature conditions of base catalyst and 70-80 ℃;
B, elevated temperature also are controlled in the 90-150 ℃ of scope, and described amino silicane coupling agent and silicone monomers are reacted in this temperature range, generate amido silicon oil and low-boiling-point substance;
C, vacuumize and distillate low-boiling-point substance;
D, reduce temperature and be controlled at 40-80 ℃ of scope, separate obtaining amido silicon oil;
E, amido silicon oil was reacted 1-5 hour under 40-120 ℃ temperature conditions with epoxychloropropane in atent solvent, generate epoxy modified amino-silicone oil;
F, removal atent solvent obtain epoxy modified amino-silicone oil;
G, epoxy modified amino-silicone oil added carry out emulsification in the emulsifying agent, and adopt weak acid that the pH value of emulsion is adjusted to 6-7, then obtain epoxy modified amino-silicone oil softening agent.
2, preparation method according to claim 1 is characterized in that, described step C specifically comprises step:
C1, under 90-150 ℃ temperature conditions, be evacuated to 0.02-0.03mpa, distillate low-boiling-point substance;
C2, gas clean-up reach in the scope of 1000-20000cs its material viscosity to 0.05-0.1mpa, and low-boiling-point substance distillates fully, stops to vacuumize.
3, preparation method according to claim 1 is characterized in that, described step F specifically may further comprise the steps:
F1, under the vacuum condition of 60-100 ℃ temperature and 0.03-0.06mpa, remove atent solvent.
4, preparation method according to claim 1, it is characterized in that described amino silicane coupling agent is one or more of following component: N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl methyldiethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane, N-cyclohexyl-y-aminopropyl methyl dimethoxysilane, γ-piperazinyl propyl group methyl dimethoxysilane.
5, preparation method according to claim 1 is characterized in that, described silicone monomers is one or more of following component: octamethylcy-clotetrasiloxane, methyl cyclosiloxane mix monomer, the linear hydroxy-end capped silicone oil of low molecular weight.
6, preparation method according to claim 1 is characterized in that, described base catalyst is a TMAH.
7, preparation method according to claim 1 is characterized in that, described atent solvent is toluene or dimethylbenzene.
8, preparation method according to claim 1 is characterized in that, described emulsifying agent is one or more of following component: alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, isomery fatty alcohol-polyoxyethylene ether.
9, preparation method according to claim 1 is characterized in that, described amino silicane coupling agent and silicone monomers mass ratio are between the 1:199-1:9.
10, preparation method according to claim 1 is characterized in that, the quality of described base catalyst accounts for the 0.3%-1% of described amino silicane coupling agent and silicone monomers quality summation.
11, preparation method according to claim 1 is characterized in that, described epoxychloropropane and amino silicane coupling agent mol ratio are between 3:10-1:1.
12, preparation method according to claim 1, other are characterised in that the mass ratio of described atent solvent and amido silicon oil is 1:10-1:1.
13, preparation method according to claim 1 is characterized in that, the mass ratio of described emulsifying agent and epoxy modified amino-silicone oil is 0.3-0.5.
14, preparation method according to claim 1 is characterized in that, the described weak acid among the described step G is acetic acid.
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