CN104862980B - Preparation method and apparition of wet rubbing fastness improver containing copper microcapsules - Google Patents
Preparation method and apparition of wet rubbing fastness improver containing copper microcapsules Download PDFInfo
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- CN104862980B CN104862980B CN201510250525.5A CN201510250525A CN104862980B CN 104862980 B CN104862980 B CN 104862980B CN 201510250525 A CN201510250525 A CN 201510250525A CN 104862980 B CN104862980 B CN 104862980B
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Abstract
The invention relates to a preparation method and an apparition of a wet rubbing fastness improver containing copper microcapsules. The preparation method comprises the following steps: (1), silane modified ultrafine copper nanopowder is prepared; (2), the ultrafine copper nanopowder is ground and dried to constant weight; (3), the dried ultrafine copper nanopowder, 2,2'-azodiisobutyronitrile, divinyl benzene, butyl acrylate, methyl methacrylate and distilled water are mixed uniformly, tricalcium phosphate is added, and the mixture is subjected to ultrasonic vibration to obtain a dispersing liquid; (4) the dispersing liquid is placed into a flask with four necks to be subjected to heating, micro-suspension polymerization, heating and curing, and a product is washed with excessive hydrochloric acid solution and then washed to neutral to obtain the wet rubbing fastness improver containing the copper microcapsules. The prepared wet rubbing fastness improver containing the copper microcapsules can improve the wearability of fabric dyed with reactive dye, and the preparation method has the characteristics of simplicity, low cost, little time and labor investment, low toxicity of synthetic raw materials and reduction of environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method and application comprising metallic copper microcapsule wet friction fastness improving agent.
Background technology
The nano materials such as copper powder, nikel powder and secret powder can be applicable to lube oil additive, can substantially reduce body surface and rub
Coefficient is wiped, wherein Nanometer Copper has good lubricating function, and has good repair function to worn-out body surface.
Ultrasound wave can produce series of effects in water transmission, after large power supersonic acts on solution, produce in solution
Liquid drawing crack is produced emptying aperture by raw negative pressure, negative pressure, and low density gas or steam are now filled with emptying aperture, cavitation nucleus is formed, in sound
Under the effect of vibration of field, when acoustic pressure reaches certain value, bubble will expand rapidly, then close suddenly, and in closure punching is produced
Ripple is hit, a series of this dynamic process is referred to as ultrasonic cavitation.Using ultrasonic cavitation can reach degasification, cavitation erosion, temperature,
The a series of effects such as dispersion.Ultrasonic disperse effect refers to ultrasonication when in liquid-liquid or liquid-solid biphase medium, it may occur that
Strong stirring action, microgranule is refined, and a kind of medium uniformly, is rapidly dispersed in another medium.At ultrasound
During reason resin colloid solution, the peptizaiton of ultrasound can be such that colloid solution concentration distribution obtains evenly.Scientist's research is sent out
Existing, than mechanical dispersion effect more preferably, colloidal particle size is less, narrow distribution for ultrasonic disperse.Microsuspension polymerization is in suspension polymerisation base
A kind of newer type polymerization developed on plinth.The method preferably maintain drop that suspension polymerisation has directly into
Core mechanism;Simultaneously by reinforcing dispersion and suspending process, particle size can be more easily controlled again in 1～20 μ m
Interior (can preferably fill up the gap of emulsion polymerization and suspension polymerisation in particle diameter distribution), therefore the polymerization is particularly well-suited to
Micro encapsulation parcel is carried out to submicron order content.
At present, the wet friction fastness improving agent on market is in the majority with polyurethane type, is primarily present following defect：First,
Wet friction fastness improving agent production cost is higher, large usage quantity, and fabric coloured light and physical and mechanical propertiess are had an impact.Second, certain
The synthesis material toxicity of a little wet friction fastness improving agents is larger, and production has potential safety hazard, does not meet environmental requirement.Such as, aqueouss
Polyurethaness wet friction fastness improving agent is with Toluene-2,4-diisocyanate, 4- diisocyanate（TDI）For synthesis material, TDI toxicity is stronger, has
Carcinogenecity.
Nano material has the nano materials such as low toxicity and advantages of environment protection, copper powder under friction condition, can rub
Wipe the surface of solids and form a smooth protection layer, reduce and rubbed between material, acted on by similar " micro- bearing ", reduce friction resistance
Power, reduces coefficient of friction.With Ni metal as main functional materials, using MOLECULE DESIGN modified metal Cu, under ultrasonic homogenizing
Metallic copper microcapsule wet friction fastness improving agent is prepared using micro-suspension polymerization.Ultrasonic homogenizing microsuspension polymerization preparation method exists
Temporarily nothing is referred in the preparation of the wet elevator that rubs.
Based on this, the present invention is proposed.
The content of the invention
For the above-mentioned technical problem of prior art, it is an object of the invention to provide a kind of rub containing the wet of copper microcapsule
The preparation method of rubbing fastness elevator, and apply on Fabrics Dyed with Reactive Dyes.The wet elevator that rubs is specifically preferably stable
Property, average volume particle diameter 3498nm, the wet friction fastness improving agent is applied can improve activity in cotton fabrics dyed with reactive dyes
Dyestuff deep-colour fabric fastness to wet rubbing, can be water-fastness in fabric face film forming.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions：
A kind of preparation method of copper microcapsule wet friction fastness improving agent, comprises the following steps：
(1) the copper superfines of silylation modification are prepared；
(2) by step（1）The copper superfines of middle preparation are through grinding, drying to constant weight；
(3) copper superfines and 2,2 '-azodiisobutyronitrile in step (2) drying, divinylbenzene, styrene, third
Olefin(e) acid butyl ester, methyl methacrylate and distilled water mix homogeneously, add tricalcium phosphate, at 25 DEG C supersonic vibration 3～
5min, obtains dispersion liquid；
(4) dispersion liquid of step (3) is put into into N270 DEG C are warming up in the four-neck flask of protection, under certain stir speed (S.S.)
Microsuspension polymerization 5h is carried out, the later stage is warming up to 95 DEG C of ripening 0.5h, polymerizate is washed with excessive hydrochloric acid solution, then be washed to
Neutrality, obtains copper microcapsule wet friction fastness improving agent.
The step（1）The preparation method of the copper superfines of middle silylation modification is：Weigh 0.05mol/L γ-shrink
Glycerol ether oxygen propyl trimethoxy silicane 100mL adds appropriate L-AA point stirring, mixing speed in four-neck flask
500 revs/min, and be warming up to 80 DEG C, measure 0.5mol/L 100～200mL of copper sulphate pentahydrate in separatory funnel, it is every at 80 DEG C
Continue stirring reaction 2～3 hours after the speed whole completion of dropping of the drop of minute 60～80, bronzing copper micropowder is obtained after cooling
End.
Described step（2）In drying temperature be 80～100 DEG C.
Described step（3）It is middle adopt for ultrasonic homogenizing under microsuspension polymerization preparation method, concretely comprise the following steps：In step
（2）Bronzing copper nano ultrafine powderses end 1.00g and the 2,2 '-azodiisobutyronitrile 0.50g of drying, divinylbenzene 0.25g, benzene
Ethylene 26.75g, butyl acrylate 20.00g, methyl methacrylate 2.50g and water mix homogeneously, add tricalcium phosphate
1.0g, distilled water 100g, supersonic vibration disperses 3min at power 800W, 25 DEG C after stirring, and obtains dispersion liquid.
A kind of application of copper microcapsule wet friction fastness improving agent on Fabrics Dyed with Reactive Dyes.
Using when the dyed fabric improve dry, 1 grade of fastness to wet rubbing.
The reactive dye are the dark blue ESP of Remazol, the red KC of Remazol or the black B of Remazol.
Beneficial effects of the present invention are as follows：
The present invention prepares the wet friction fastness improving agent containing copper microcapsule using ultrasonic homogenizing microsuspension polymerization method, closes
It is relatively low into material toxicity, have fewer environmental impacts.
The concrete preferably stability of the copper microcapsule wet friction fastness improving agent of the present invention, average volume particle diameter 1000-
It is preferable in fabric face film property between 4000nm scopes.
Copper microcapsule wet friction fastness improving agent of the present invention is applied in reactive dye, can be carried on deep colour dyeing bafta
High dark blue, red, black and active dye deep-colour fabric fastness to wet rubbing, wet friction finishing agent is firmly combined with fabric, to knitting
Light is looked for affect less.
The present invention improves the wearability of Reactive Dyes in Deep Shade fabric, and simple with method, with low cost, the time
It is few with human input, synthesis material small toxicity, and the characteristics of reduce environmental pollution.
Description of the drawings
Fig. 1 is the scanning electron microscope diagram of copper microcapsule wet friction fastness improving agent prepared by the present invention；
Fig. 2 is the grain size distribution of copper microcapsule wet friction fastness improving agent prepared by the present invention；
Fig. 3 is fabric face scanning electron microscope before copper microcapsule wet friction fastness improving agent prepared by the present invention is arranged
Figure；
Fig. 4 is fabric face scanning electron microscope after copper microcapsule wet friction fastness improving agent prepared by the present invention is arranged
Figure.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
Embodiment 1
The preparation of the copper microcapsule wet friction fastness improving agent of the present embodiment 1, comprises the following steps：
（1）0.05mol/L γ-glycidyl ether oxygen propyl trimethoxy silicane 100mL is weighed in four-neck flask, is added
8.8gL- ascorbic acid is sufficiently stirred for（500 revs/min of mixing speed）And it is warming up to 80 DEG C, measure 0.5mol/L copper sulphate pentahydrate
200mL continues stirring reaction 3 hours, cooling at 80 DEG C in separatory funnel after the speed whole completion of dropping of 60 drop per minute
After obtain bronzing copper nano ultrafine powderses end 3.20g, in the reaction all medicines be analysis it is pure, water used be distilled water；
（2）By step（1）The bronzing copper nano ultrafine powderses end of middle collection, is ground, and distilled water wash 2 times is rearmounted
In 85 DEG C of drying 2h of baking oven；
（3）In step（2）Bronzing copper nano ultrafine powderses end 1.00g and the 2,2 '-azodiisobutyronitrile 0.50g of drying,
Divinylbenzene 0.25g, styrene 26.75g, butyl acrylate 20.00g, methyl methacrylate 2.50g and water mixing are
It is even, tricalcium phosphate 1.0g, distilled water 100g are added, the supersonic vibration at 25 DEG C after stirring（Power 800W）Dispersion
3min, obtains corresponding dispersion liquid；Water used is distilled water；
（4）By step（3）Dispersion liquid is put into N270 DEG C are warming up in the four-neck flask of protection, necessarily stir under speed being mixed
250 turns/min, microsuspension polymerization 5h is carried out, 95 DEG C of ripening 0.5h are warming up to after terminating, by polymerizate 500mL 0.1mol/
L hydrochloric acid solutions are washed, then are washed three times with 500 mL distilled water, have obtained copper microcapsule wet friction fastness improving agent.
Embodiment 2
The preparation of the copper microcapsule wet friction fastness improving agent of the present embodiment 2, comprises the following steps：
（1）0.05mol/L γ-glycidyl ether oxygen propyl trimethoxy silicane 100mL is weighed in four-neck flask, is added
8.8gL- ascorbic acid is sufficiently stirred for（500 revs/min of mixing speed）And it is warming up to 80 DEG C, measure 0.5mol/L copper sulphate pentahydrate
200mL continues stirring reaction 3 hours, cooling at 80 DEG C in separatory funnel after the speed whole completion of dropping of 60 drop per minute
After obtain bronzing copper nano ultrafine powderses end 3.20g, in the reaction all medicines be analysis it is pure, water used be distilled water；
（2）By step（1）The bronzing copper nano ultrafine powderses end of middle collection, is ground, and distilled water wash 2 times is rearmounted
In 85 DEG C of drying 2h of baking oven；
（3）In step（2）Bronzing copper nano ultrafine powderses end 2.00g and the 2,2 '-azodiisobutyronitrile 1.00g of drying,
Divinylbenzene 0.50g, styrene 53.50g, butyl acrylate 40.00g, methyl methacrylate 5.00g and water mixing are
It is even, tricalcium phosphate 2.0g, distilled water 200g are added, the supersonic vibration at 25 DEG C after stirring（Power 600W）Dispersion
3min, obtains corresponding dispersion liquid；Water used is distilled water；（4）By step（3）Emulsion be put in four-neck flask and be warming up to
React 5 hours after 70 DEG C, 95 DEG C of ripening 0.5h are warming up to after terminating, polymerizate is washed with 500mL 0.1mol/L hydrochloric acid solutions
Wash, then washed three times with 500 mL distilled water, obtained copper microcapsule wet friction fastness improving agent.
Performance test
The particle diameter of the copper microcapsule wet friction fastness improving agent prepared to embodiment 1 and embodiment 2, viscosity, solid content enter
Row test, particle diameter test result is shown in Fig. 1.
The copper microcapsule wet friction fastness improving agent for being prepared embodiment 1 and embodiment 2 using padding method is applied in activity
On dyeing bafta, wet friction fastness improving agent 40g/L, pH6.0, one immersing and rolling, liquid carrying rate 100%, drying temperature 80
DEG C, 2min bakes 110 DEG C, 2min.Fabric property is shown in Table 1 before and after wet friction fastness improving agent performance and arrangement.By Fig. 1 and Biao 1
Understand, the ecological copper wet friction fastness improving agent average volume particle diameter of embodiment 1 and embodiment 2 in respectively 2492,3498nm,
Viscosity is respectively 17.2,16.5mPaS, and solid content reaches more than 30%, meets the performance of textile auxiliary.
The copper microcapsule wet friction fastness improving agent of embodiment 1 and embodiment 2 is applied in cotton fabrics dyed with reactive dyes
On, fabric face form, the fastness to wet rubbing of dyed fabric are tested respectively before and after the distribution, arrangement to elevator,
As a result as shown in Figure 2, Figure 3, Figure 4.Fabric abrasive fastness is shown in Table 1 before and after arrangement.
Bafta K/S values and crock fastness before and after the arrangement of table 1.
Note：1st, the red KC dyeing concentrations of the dark blue ESP of Remazol, Remazol are 6%owf, and the black B dyeing concentrations of Remazol are 8%
owf；2nd, by the dry of GB/T3920-1997 standard testing dyed cotton fabrics, fastness to wet rubbing.
From the present embodiment 1 and 2 it can be seen that the copper microcapsule wet friction fastness improving agent average volume particle diameter for preparing exists
Between 1000-4000nm scopes, metallic copper, with obvious microencapsulated forms, is assembled in aqueous in spherical in " Punica granatum L. shape ",
Its viscosity and solid content reach the requirement of textile auxiliary.From corresponding SEM photograph, elevator can dyed fabric surface into
Film, film surface is smooth, and yam surface pit-hole is less, reverses and disappears, and copper microgranule is preferably embedded in acrylate, silane
Base modification Cu microgranules have good anti-attrition, lubricating function, it is possible to decrease body surface coefficient of friction, so as to improve dyed fabric
Fastness to wet rubbing.The wet elevator that rubs is combined uniformly with fabric, can improve 1 grade of Fabrics Dyed with Reactive Dyes fastness to wet rubbing.
The present invention prepares a kind of wet friction fastness improving agent containing copper microcapsule, and synthesis material toxicity is relatively low, to environment
Affect less.The wet elevator specifically preferable stability of rubbing, between average volume particle diameter 1000-4000nm scopes, in fabric
Surface filming is preferable.Secondly the wet elevator that rubs of the present invention being applied can improve Tibetan on Reactive Dyes in Deep Shade bafta
Blue or green, red, 1 grade of the fastness to wet rubbing of black and active dye deep-colour fabric, wet friction finishing agent is firmly combined with fabric, to fabric
Coloured light affects less.The present invention improves the wearability of Fabrics Dyed with Reactive Dyes, and simple with method, with low cost, when
Between and human input it is few, synthesis material small toxicity, and the characteristics of reduce environmental pollution.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention,
All changes for carrying out unsubstantiality to the present invention using this design, all should fall into protection scope of the present invention.
Claims (7)
1. a kind of preparation method of copper microcapsule wet friction fastness improving agent, it is characterised in that comprise the following steps：
(1) the copper superfines of silylation modification are prepared；
(2) by step（1）The copper superfines of middle preparation are through grinding, drying to constant weight；
(3) in the copper superfines and 2,2 '-azodiisobutyronitrile, divinylbenzene, styrene, acrylic acid of step (2) drying
Butyl ester, methyl methacrylate and distilled water mix homogeneously, add tricalcium phosphate, and 3～5min of supersonic vibration, obtains at 25 DEG C
To dispersion liquid；
(4) dispersion liquid of step (3) is put into into N270 DEG C are warming up in the four-neck flask of protection, are carried out under certain stir speed (S.S.)
Microsuspension polymerization 5h, the later stage is warming up to 95 DEG C of ripening 0.5h, and polymerizate is washed with excessive hydrochloric acid solution, then in being washed to
Property, obtain copper microcapsule wet friction fastness improving agent.
2. the preparation method of copper microcapsule wet friction fastness improving agent as claimed in claim 1, it is characterised in that the step（1）
The preparation method of the copper superfines of middle silylation modification is：Weigh 0.05mol/L γ-glycidyl ether oxygen propyl trimethoxy
Base silane 100mL adds the stirring of appropriate L-AA, 500 revs/min of mixing speed in four-neck flask, and is warming up to 80
DEG C, 0.5mol/L 100～200mL of copper sulphate pentahydrate are measured in separatory funnel, the speed of 60～80 drop per minute is complete at 80 DEG C
Continue stirring reaction 2～3 hours after portion's completion of dropping, bronzing copper superfines are obtained after cooling.
3. the preparation method of copper microcapsule wet friction fastness improving agent as claimed in claim 1, it is characterised in that：Described step
（2）In drying temperature be 80～100 DEG C.
4. the preparation method of copper microcapsule wet friction fastness improving agent as claimed in claim 1, it is characterised in that：Described step
（3）It is middle adopt for ultrasonic homogenizing under microsuspension polymerization preparation method, concretely comprise the following steps：In step（2）The bronzing copper of drying
Nano ultrafine powderses end 1.00g and 2,2 '-azodiisobutyronitrile 0.50g, divinylbenzene 0.25g, styrene 26.75g, acrylic acid
Butyl ester 20.00g, methyl methacrylate 2.50g and water mix homogeneously, add tricalcium phosphate 1.0g, distilled water 100g, stirring
Supersonic vibration disperses 3min at power 800W, 25 DEG C after uniform, obtains dispersion liquid.
5. the copper microcapsule that a kind of preparation method of copper microcapsule wet friction fastness improving agent as claimed in claim 4 is prepared
Application of the wet friction fastness improving agent on Fabrics Dyed with Reactive Dyes.
6. application of the copper microcapsule wet friction fastness improving agent as claimed in claim 5 on Fabrics Dyed with Reactive Dyes, its
It is characterised by：Using when the dyed fabric improve dry, 1 grade of fastness to wet rubbing.
7. application of the copper microcapsule wet friction fastness improving agent as claimed in claim 5 on Fabrics Dyed with Reactive Dyes, its
It is characterised by：The reactive dye are the dark blue ESP of the Remazol or black B of Remazol.
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| CN107268307A (en) * | 2017-06-07 | 2017-10-20 | 常州中翔科技有限公司 | A kind of wet friction fastness improving agent for dyeing fabric |
| CN107265886A (en) * | 2017-06-07 | 2017-10-20 | 常州市海若纺织品有限公司 | A kind of epoxy resin modification starch film forming agent |
| CN108221375A (en) * | 2017-12-11 | 2018-06-29 | 江苏新瑞贝科技股份有限公司 | A kind of preparation method of dry wet friction fastness improving agent |
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| US5821177A (en) * | 1996-12-16 | 1998-10-13 | Trichromatic Carpet Inc. | Enhancement of stain resistance or acid dye fixation, improved light fastness and durability of fibrous poolyamide and wool substrates |
| CN101503860A (en) * | 2008-02-04 | 2009-08-12 | 上海德桑精细化工有限公司 | Wet friction fastness improving agent for dyeing fabric |
| CN101608407A (en) * | 2009-07-04 | 2009-12-23 | 金根苗 | A kind of production technology that improves wet rubbing fastness of reactive dye |
| CN102941046A (en) * | 2012-11-26 | 2013-02-27 | 天津工业大学 | Preparation method for micro/nano-capsule with metal ion complex capsule wall |
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|---|---|---|---|---|
| US5821177A (en) * | 1996-12-16 | 1998-10-13 | Trichromatic Carpet Inc. | Enhancement of stain resistance or acid dye fixation, improved light fastness and durability of fibrous poolyamide and wool substrates |
| CN101503860A (en) * | 2008-02-04 | 2009-08-12 | 上海德桑精细化工有限公司 | Wet friction fastness improving agent for dyeing fabric |
| CN101608407A (en) * | 2009-07-04 | 2009-12-23 | 金根苗 | A kind of production technology that improves wet rubbing fastness of reactive dye |
| CN102941046A (en) * | 2012-11-26 | 2013-02-27 | 天津工业大学 | Preparation method for micro/nano-capsule with metal ion complex capsule wall |
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