CN104086779A - Super-soft/smooth block silicon oil and preparation method thereof - Google Patents
Super-soft/smooth block silicon oil and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of textile finishing agents, particularly a super-soft/smooth block silicon oil and a preparation method thereof. The preparation method comprises the following steps: after mixing octamethylcyclotetrasiloxane and an amino coupling agent, reacting under the action of an alkaline catalyst to obtain a common side chain amino modified silicon oil intermediate A; reacting the prepared A with an amino-terminated polyether coupling agent under the action of an alkaline catalyst to obtain an amino-terminated polyether block and side chain amino modified silicon oil intermediate B; and carrying out polymerization reaction on the prepared B and epoxy-terminated polyether under the action of an organic solvent to finally obtain terpolymer block side chain amino-modified organic silicon oil. By introducing side chain amino group into the straight-chain terpolymer block silicon oil compound, the fabric finished by the compound has excellent soft, fluffy and smooth effects and excellent whiteness, and thus, the compound is suitable for super-soft/smooth finishing of cotton, cotton-chemical fiber blend fabrics and the like.
Description
Technical field
The present invention relates to sliding block silicone oil of a kind of ultra-soft and preparation method thereof, the flexible smooth being mainly used in after-finishing of textile products process arranges.
Background technology
At present, during the various amino-modified silicone oil emulsions of take are that rear arrangement that main softening agent is widely used in the textiless such as cotton, silk, wool and terylene is processed, the fabric of arrangement has softness, characteristic smooth, attractive in appearance, washable and comfortable and easy to wear.This series products is accepted by people.The fabric that weak point is mainly manifested in through its arrangement is hydrophobicity; The light color and the white fabrics that with it, arrange, after high temperature bakes, there will be Yellowing in various degree, and the stability of a lot of amino-modified silicone emulsions is very poor, in be everlasting storage and application process, occurs breakdown of emulsion floating oil phenomenon; In padding use procedure, there is roll banding phenomenon to produce.
In order to overcome the above-mentioned shortcoming of traditional amido silicon oil, people adopt the whole bag of tricks to improve, and have side chain polyether-modified, also have epoxide modifiedly or carboxy-modified, and silicone oil stability after modification improves, but feel deviation.The later stage nineties 20th century, the people such as the A.M.Czech of company of Yuan Wei section propose to carry out amino and the copolymerization of polyether-based linearity block siloxane backbone from the angle of molecular designing, synthetic new linear amino-polyether group block copolymer, be better than amino anchorage effect, make whole polysiloxane can firmly be combined in fabric face, the flexible smooth that has kept polysiloxane crude oil, hydrophilic polyether segment is present in fiber surface to fall the form of shape, water molecules is in the uncrossed transmission of fiber surface, form soft and hydrophilic compatibility, this is that silicone softening agent develops to obtain a new stage, also be following developing direction.
Current flexible smooth agent is on the market used for the fabrics such as cotton textiles, purifying fibre, and flexible smooth finishing composition effect in BLENDED FABRIC is all general, its flexibility, smoothness, rebound resilience are all poor, and domestic addressing this problem mostly adopts composite mode, but it is more complicated, and DeGrain.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, a kind of super flexible smooth terpolymer of BLENDED FABRIC block silicone oil that is applicable to the fibers such as cotton and cotton and chemical fibre and preparation method thereof is provided
In order to achieve the above object, the technical solution used in the present invention is: in straight chain terpolymer block silicon oil compound, introduce side chain amino, thereby make the fabric after such compound treatment have the effect of soft fluffy more, this method comprises following step:
1) side chain amino-modified silicone oil intermediate is synthetic
By after octamethylcyclotetrasiloxane and amino coupling agent mixing, under the effect of basic catalyst, react, obtain common side chain amino-modified silicone oil intermediate;
2) prepare Amino Terminated polyether(ATPE) block silicone intermediate
By 1) prepared common side chain amino-modified silicone oil intermediate reacts under basic catalyst with Amino Terminated polyether(ATPE) coupling agent,, make Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate;
3) preparation of finished product
By 2) prepared Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate carry out polyreaction with end epoxidized polyether under the effect of organic solvent, finally obtains the amino modified organic silicone oil of terpolymer block side chain.
As further improvement, step 1) described octamethylcyclotetrasiloxane and the mass ratio of amino coupling agent be 100:1-100:3, the reaction times is 3-4h.
As further improvement, step 1) described amino coupling agent is one or more mixtures in γ-piperazinyl propyl group methyl dimethoxysilane, γ-diethylenetriamine propyl group methyl dimethoxysilane, N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane.
As further improvement, step 2) described Amino Terminated polyether(ATPE) coupling agent is that structural formula is:
Wherein R is-CH
2-CH
2-and-CH
2-CH
2(CH
3)-in any one or two combinations, m, n=1～10;
As further improvement, step 2) reaction conditions under basic catalyst effect described in is: when catalyzer is potassium hydroxide, temperature of reaction is 140-145 ℃, reaction times is 3-4h, and when catalyzer is Tetramethylammonium hydroxide, temperature of reaction is 110-120 ℃, and the reaction times is 3-4h.
As further improvement, step 2) molecular weight of described Amino Terminated polyether(ATPE) coupling agent is one or more mixtures of 300,500,600,800,1000.
As further improvement, step 2) the mass ratio 100:5-100:10 of described side chain amino-modified silicone oil intermediate and end group polyetheramine coupling agent.
As further improvement, step 3) described organic solvent is one or more mixture of Virahol, ethylene glycol monobutyl ether, ethylene glycol ether, ethylene glycol monomethyl ether, Diethylene Glycol, dipropylene glycol.
As further improvement, step 3) molecular structural formula of described end epoxidized polyether is:
Wherein, a=0-3, b=0-3, one or more end epoxidized polyethers in n=6-85.
As further improvement, step 3) molecular weight of described end epoxidized polyether one or more mixtures that are 400-4000.
As further improvement, step 3) described Amino Terminated polyether(ATPE) modified silicon oil intermediate, end epoxidized polyether mass ratio be 100:10-100:20
The sliding block silicone oil of ultra-soft that a kind of method described in use makes.
After adopting technical scheme of the present invention, with respect to prior art, have the following advantages:
The refreshing block silicone oil of superslide prepared by the present invention take domesticly easily produce, easily buying, material various in style are basic material, in straight chain terpolymer block silicon oil compound, successfully introduce side chain amino, fabric has the smooth effect of splendid soft fluffy and whiteness after using this compounds to arrange, and the super flexible smooth that is applicable to the fiber mixed fabrics such as cotton, cotton and chemical fibre arranges.In addition, this compounds emulsion is also had a satisfactory stability, solved traditional amido silicon oil easy breakdown of emulsion, floating oil, roll banding, sticky cylinder, easily produce oil mark, the problem such as be difficult for returning something for repairs.
Specific embodiment
Embodiment 1:
The first step, octamethylcyclotetrasiloxane and amino coupling agent are dropped in reactor by 100:1 (mass ratio) in proportion, stir and heat up, be heated to 80-85 ℃, add and account for the potassium hydroxide aqueous solution that total mass 0.02% concentration is 30%, continue to be warming up to 140-145 ℃, insulation 3-4h, then be cooled to 120 ℃ and vacuumized low molecular weight substance, obtain water white transparency dope, be side chain amino-modified silicone oil intermediate; Second step, side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent are dropped in reactor in 100:8 (mass ratio) ratio, be heated to 80-85 ℃, add the potassium hydroxide aqueous solution that side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent quality 0.1% concentration are 30%, continue to be warming up to 140-145 ℃, insulation 3-4h, then be cooled to 120 ℃ and vacuumized low molecular weight substance, obtain yellow transparent dope, be Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate; The 3rd step, Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate drop into reactor with end epoxidized polyether according to the ratio of 100:10 (mass ratio), the Virahol that adds again total mass 40%, at 80 ℃, react 6h, obtain light yellow transparent liquid, i.e. terpolymer side chain amino-modified silicone oil A.
Embodiment 2:
The first step, octamethylcyclotetrasiloxane and amino coupling agent are dropped in reactor by 100:3 (mass ratio) in proportion, stir and heat up, be heated to 80-85 ℃, add the Tetramethylammonium hydroxide that accounts for total mass 0.02%, continue to be warming up to 110-120 ℃, insulation 3-4h, then be warming up to 145 ℃ and vacuumize and remove low-boiling-point substance and catalyzer, obtain water white transparency dope, be side chain amino-modified silicone oil intermediate; Second step, side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent are dropped in reactor in 100:5 (mass ratio) ratio, be heated to 80-85 ℃, the Tetramethylammonium hydroxide that adds side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent quality 0.1%, continue to be warming up to 110-120 ℃, insulation 3-4h, then being warming up to 145 ℃ vacuumizes and removes low-boiling-point substance and catalyzer, obtain yellow transparent dope, be Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate; The 3rd step, Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate drop into reactor with end epoxidized polyether according to the ratio of 100:20 (mass ratio), the ethylene glycol monobutyl ether that adds again total mass 40%, at 120 ℃, react 6h, obtain yellow transparent liquid, i.e. terpolymer side chain amino-modified silicone oil B.
Embodiment 3:
The first step, octamethylcyclotetrasiloxane and amino coupling agent are dropped in reactor by 100:2 (mass ratio) in proportion, stir and heat up, be heated to 80-85 ℃, add the Tetramethylammonium hydroxide that accounts for total mass 0.02%, continue to be warming up to 110-120 ℃, insulation 3-4h, then be warming up to 145 ℃ and vacuumize and remove low-boiling-point substance and catalyzer, obtain water white transparency dope, be side chain amino-modified silicone oil intermediate; Second step, side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent are dropped in reactor in 100:10 (mass ratio) ratio, be heated to 80-85 ℃, the Tetramethylammonium hydroxide that adds side chain amino-modified silicone oil intermediate and Amino Terminated polyether(ATPE) coupling agent quality 0.1%, continue to be warming up to 110-120 ℃, insulation 3-4h, then being warming up to 145 ℃ vacuumizes and removes low-boiling-point substance and catalyzer, obtain yellow transparent dope, be Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate; The 3rd step, Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate drop into reactor with end epoxidized polyether according to the ratio of 100:15 (mass ratio), add again total mass 40% ethylene glycol monobutyl ether, at 120 ℃, react 6h, obtain yellow transparent liquid, i.e. terpolymer side chain amino-modified silicone oil C.
To embodiment 1, embodiment 2 and the embodiment 3 product ternary of producing, side chain amino-modified silicone oil A, B and C carry out the detection of the contrast of effect and xanthochromia, stability altogether.
1. the preparation of finishing composition
Terpolymer side chain amino-modified silicone oil A, B and C adopt TO series emulsifying agent to carry out emulsification, the ratio of oil and emulsifying agent
10:1 ?15:1 (mass ratio), after emulsification, product appearance is colourless transparent liquid.
2. the application art of finishing composition
Process fabric: terylene sheeting (specification is T/C65/3532*32/130*70)
Treatment process: consumption 50g/L, normal temperature one soaks one and rolls the qualitative oven dry of (pick-up 70-75%) → 180 ℃ * 2min; Fabric after arrangement, after the 24h of balance moisture regain at normal temperatures, carries out performance evaluation;
3. result contrast
3.1 feel testing method:
Through 5 experienced feel experts, from aspect comprehensive evaluations such as slippery, elasticity and pliabilitys, what feel was best is 5 minutes, and former cloth feel is 1 minute, finally averages to determine evaluation result, and test result is in Table 1.
3.2 xanthochromia testing method
Adopt padding method, silicone oil emulsion is processed on polyester-cotton blend brightened goods, and the whiteness value with fabric after COLOR-EYE3100 tester test untreated (former cloth) and processing, then contrasts.Tested fabric whiteness value is less, and xanthochromia is larger, and test result is in Table 1.
3.3 environment and composite stability test method
Organic silicon emulsion is tested at different pH and with the stability in the composite situation of other auxiliary agents.Solution usage 20g/L to be measured, adds other reagent to stir, and observes solution state and change after placement 4h, and test result is in Table 2.
3.3 resistance to shear stability testing method
Get silicon oil solution to be sheared (solid content 10%-20%) 200g/L, on high speed shear instrument, whether with 3000 turn/min high speed shear 30min, having sheared rear placement 24h observation solution has floating oil and breakdown of emulsion to occur, test result is in Table 2.
Table 1 feel and whiteness result
Table 2 stability result
Data by table 1, table 2 can be found out, the fabric that adopts super soft and smooth block silicone oil to process, has excellent flexible smooth feel, good whiteness and stability, be widely used field and wide application prospect can thoroughly replace common terpolymer amido silicon oil comprehensively.
Claims (10)
1. ultra-soft is slided a preparation method for block silicone oil, and this synthetic method comprises the following steps:
A prepares common side chain amino-modified silicone oil intermediate
By after octamethylcyclotetrasiloxane and amino coupling agent mixing, under the effect of basic catalyst, reaction obtains common side chain amino-modified silicone oil intermediate;
B prepares Amino Terminated polyether(ATPE) block silicone intermediate
Adopt prepared common side chain amino-modified silicone oil intermediate in steps A to react under basic catalyst effect with Amino Terminated polyether(ATPE) coupling agent, make Amino Terminated polyether(ATPE) block and side chain amino-modified silicone oil intermediate;
The preparation of C finished product
Prepared Amino Terminated polyether(ATPE) block in step B and side chain amino-modified silicone oil intermediate are carried out to polyreaction with end epoxidized polyether under the effect of organic solvent, finally obtain the amino modified organic silicone oil of terpolymer block side chain.
2. the preparation method of the sliding block silicone oil of ultra-soft according to claim 1, is characterized in that: the amino coupling agent described in steps A is one or more mixtures in γ-piperazinyl propyl group methyl dimethoxysilane, γ-diethylenetriamine propyl group methyl dimethoxysilane, N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxysilane.
3. the preparation method of the sliding block silicone oil of ultra-soft according to claim 1, is characterized in that: the mass ratio of the octamethylcyclotetrasiloxane described in steps A and amino coupling agent is 100:1-100:3, and the reaction times is 3-4h.
4. ultra-soft according to claim 1 is slided the preparation method of block silicone oil, it is characterized in that: the Amino Terminated polyether(ATPE) coupling agent described in step B is that structural formula is:
Wherein R is-CH
2-CH
2-and-CH
2-CH
2(CH
3)-in any one or two combinations, m, n=1～10.
5. ultra-soft according to claim 1 is slided the preparation method of block silicone oil, it is characterized in that: the reaction conditions under basic catalyst effect described in step B is: when catalyzer is potassium hydroxide, temperature of reaction is 140-145 ℃, reaction times is 3-4h, when catalyzer is Tetramethylammonium hydroxide, temperature of reaction is 110-120 ℃, and the reaction times is 3-4h.
6. ultra-soft according to claim 1 is slided the preparation method of block silicone oil, it is characterized in that: the mass ratio 100:5-100:10 of the side chain amino-modified silicone oil intermediate described in step B and Amino Terminated polyether(ATPE) coupling agent, the molecular weight of Amino Terminated polyether(ATPE) amine coupling agent is one or more mixtures of 300,500,600,800,1000.
7. the preparation method of the sliding block silicone oil of ultra-soft according to claim 1, is characterized in that: the organic solvent described in step C is one or more mixture of Virahol, ethylene glycol monobutyl ether, ethylene glycol ether, ethylene glycol monomethyl ether, Diethylene Glycol, dipropylene glycol.
8. ultra-soft according to claim 1 is slided the preparation method of block silicone oil, it is characterized in that: one or more mixtures that the molecular weight of the end epoxidized polyether described in step C is 400-4000, and molecular structural formula is:
Wherein, a=0-3, b=0-3, one or more end epoxidized polyethers in n=6-85.
9. the preparation method of the sliding block silicone oil of ultra-soft according to claim 1, is characterized in that: the mass ratio of the Amino Terminated polyether(ATPE) modified silicon oil intermediate described in step C, end epoxidized polyether is 100:10-100:20.
10. the ultra-soft being made by the method described in any one in claim 1 to 9 is slided block silicone oil.
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