CN104589444B - Alkaline silica sol color fixing agent and preparation method thereof - Google Patents
Alkaline silica sol color fixing agent and preparation method thereof Download PDFInfo
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- CN104589444B CN104589444B CN201410802774.6A CN201410802774A CN104589444B CN 104589444 B CN104589444 B CN 104589444B CN 201410802774 A CN201410802774 A CN 201410802774A CN 104589444 B CN104589444 B CN 104589444B
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- fixing agent
- silica sol
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- color fixing
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/02—Staining or dyeing wood; Bleaching wood
Abstract
The invention discloses a kind of alkaline silica sol color fixing agent and preparation method thereof, alkaline silica sol color fixing agent is with tetraethyl orthosilicate, water, alcohol, catalyst and silane coupler as raw material, according to mol ratio be 1: 30～40: 20～30: 0.3～0.7: 0.001～0.01 mix after, prepared by solgel reaction；Its preparation method is: tetraethyl orthosilicate and alcoholic solvent is mixed, stirs, be made into solution A；Water is mixed homogeneously with catalyst, is made into B solution；Take 30wt%A solution in reactor, it is warming up to 30～60 DEG C, under agitation the solution A of B solution and residue 70wt% is added drop-wise in reactor, with 30～60 DEG C of condensing refluxes, after reaction 30min, drip silane coupler again, continue stirring reaction 0.5～3h, be aged 8～12h, complete the preparation of alkaline silica sol color fixing agent, there is safety and environmental protection, colour fixation strong, the advantage such as silica sol granule particle diameter is little, narrow distribution.
Description
Technical field
The present invention relates to color fixing agent technical field, particularly relate to a kind of alkaline silica sol color fixing agent and preparation method thereof.
Background technology
After timber reactive dyeing is reactive dyestuff molecule adsorption and permeation in wood, utilize the reactivity in reactive dyestuff molecule
Active group is combined with covalent bond with timber, set process in wood, is that artificial forest fast growing wood is carried out coloring treatment, system
Produce color, texture and other physical and mechanical property and meet or exceed preferable rare tree timber, improve artificial forest fast growing wood attached
Value added, it is achieved the method for processing wooden piece efficiently utilized of artificial forest fast growing wood.
After timber reactive dyeing, although owing to the absorption of amount of activated dyestuff on lumber fibre surface but is not sent out with lumber fibre
Biochemical bond is closed, and these reactive dye not being bonded with lumber fibre may fade so that the degree of fixation of timber, color fastness,
Particularly rub resistance and color fastness to washing is poor.In order to solve reactive dye degree of fixation on timber, colour fastness to rubbing and resistance to
Wash the problem that color fastness is poor, use color fixing agent to improve reactive dye degree of fixation on timber and color fastness just becomes one and has
Effect approach.Although traditional color fixing agent soda can improve the color fastness of timber, but its strong basicity can make 20～40% reactive dye
Hydrolyze, make reactive dye react with lumber fibre and form the probability reduction that covalent bond is combined；Hydrolised dye is easy simultaneously
Adsorb at wood surface, form polymolecular laminar associated complex, hinder absorption further and the diffusion of dye molecule, produce loose colour,
Not only make degree of fixation, color fastness improve degree little, more increase the weight of the consumption of water and the pollution of environment；It is simultaneously introduced substantial amounts of pure
Alkali makes in dyeing waste water containing substantial amounts of inorganic salt, the difficulty of aggravation Dyeing and Printing Wastewater Biological Treatment.Textile industry uses relatively
Many color fixing agent substitute alkali Y also can improve the color fastness of timber, but due in Y content of formaldehyde higher, have a strong impact on health,
Cause environmental pollution.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that a kind of safety and environmental protection, can significantly improve timber
The alkaline silica sol color fixing agent of dye fixing effect, also provides for a kind of preparation technology simply, easily operate, reacts controlled and silicon is molten
Glue grain diameter is little, the preparation method of the alkaline silica sol color fixing agent of narrow distribution.
For solving above-mentioned technical problem, it is provided that a kind of alkaline silica sol color fixing agent, aforementioned base Ludox color fixing agent is with positive silicic acid
Ethyl ester, water, alcohol, catalyst and silane coupler are raw material, are 1: 30～40: 20～30: 0.3～0.7 according to mol ratio:
After 0.001～0.01 mixes, prepared by sol gel reaction.
Aforesaid alkaline silica sol color fixing agent, further, the viscosity of aforementioned base Ludox color fixing agent be 25mPa S～
35mPa S, solid content is 10%～15%, and silica dioxide granule mean diameter is 10nm～20nm.
As total technology design, present invention also offers aforesaid alkaline silica sol color fixing agent preparation method, including following
Step:
(1) tetraethyl orthosilicate and alcoholic solvent are mixed, stir, be made into solution A；
(2) water is mixed homogeneously with catalyst, is made into B solution；
(3) take the aforementioned solution A of 30wt% in reactor, be warming up to 30 DEG C～60 DEG C, under agitation by molten for aforementioned B
The solution A of liquid and residue 70wt% is added drop-wise in reactor, with 30 DEG C～60 DEG C of condensing refluxes, after reaction 30min, then drips
Silane coupler, continues stirring reaction 0.5h～3h, is aged 8h～12h, completes the preparation of alkaline silica sol color fixing agent.
Aforesaid preparation method, further, is added drop-wise to reaction by the solution A of B solution and residue 70wt% in step (3)
Rate of addition in device is 1mL/min～2mL/min.
Aforesaid preparation method, further, in step (3), mixing speed is 400 turns/min～800 turns/min.
Aforesaid preparation method, further, aforementioned alcoholic solvent is dehydrated alcohol, propanol, isopropanol, the tert-butyl alcohol and n-butyl alcohol
In the mixture of one or more.
Aforesaid preparation method, further, aforementioned silane coupling agent be γ aminopropyl Ethoxysilane, N-(β-aminoethyl)-γ-
One or many in aminopropyl dimethoxy silane, VTES and vinyl-('beta '-methoxy ethyoxyl) silane
The mixture planted.
Aforesaid preparation method, further, Above-mentioned catalytic agent is ammonia.Preferably, the mass percent concentration of ammonia be 25%～
28%.
Compared with prior art, it is an advantage of the current invention that:
(1) the alkaline silica sol color fixing agent that the present invention provides is silicon dioxide colloid microgranule uniform divergent contour in water or other solvents
The colloid solution become, silica particles contains substantial amounts of hydroxyl, can improve wettability, and have bigger reactivity,
The most woven industry be widely used as the later stage process finishing agent use, netted particle membrane can be formed at fiber surface, reach fixation,
The purpose of flat wrinkle.
(2) the alkaline silica sol color fixing agent of the present invention is low viscous colloid solution, good dispersion, can be sufficiently submerged in and be filled to admittedly
In body thing, particularly porous material, and its surface is made to smooth.
(3) the alkaline silica sol color fixing agent of the present invention has good cementability, can form firm film by being dried, not only become
Film temperature is relatively low, and once film forming would not be re-dissolved in water and rotten.
(4) preparation technology of the alkaline silica sol color fixing agent that the present invention provides simply, easily operate, reacts controlled and Ludox
Grain particle diameter is little, silica dioxide granule size is generally 1～100nm, narrow distribution.
(5) the alkaline silica sol color fixing agent of the present invention is when timber reactive dyeing, and on the one hand timber is at alkaline silica sol
After reason, the gel particles on lumber fibre promotes the more upper dye of reactive dye absorption；The most small gel particles has
Specific surface area and higher specific surface energy greatly, easily forms one layer of oxide with tridimensional network at wood surface thin
Film, this tunic, by reactive dye three-dimensional set, reaches to improve stained wood fastness to rubbing and the effect of color fastness to washing.With this
When the alkaline silica sol color fixing agent of invention preparation replaces tradition color fixing agent, it is not necessary to transformation conventional reactive dyeing equipment, can drop
The use of inorganic salt or completely dispense with in low traditional handicraft, alleviates the difficulty of the pollution to environment and Dyeing and Printing Wastewater Biological Treatment, real
Existing environmental protection less salt timber reactive dyeing；And alcoholic solvent can be recycled recycling in color fixing agent, it is achieved resource reclaim
Recycling, saves production cost；The sol-gel particle simultaneously prepared with the silane coupler containing Long carbon chain can give stained wood
Waterproof, moistureproof performance.
Detailed description of the invention
Below in conjunction with concrete preferred embodiment, the invention will be further described, but protection model not thereby limiting the invention
Enclose.
Material and instrument employed in following example are commercially available.
Embodiment 1:
The preparation method of the alkaline silica sol of the present invention, specifically includes following steps:
(1) 21.2g tetraethyl orthosilicate and 92g dehydrated alcohol are mixed, stir, be made into solution A.
(2) 76g distilled water and the strong aqua ammonia that 7mL mass fraction is 28% are mixed to get B solution.
(3) solution A taking 38g puts into reactor, is warming up to 40 DEG C with 2 DEG C/min programming rate, starts in reactor
Agitator, controlling mixing speed is 500 turns/min；Rate of addition drip with 2mL/min add B solution and remaining A is molten
Liquid, with 40 DEG C of condensing refluxes, after reaction 30min, then drips the KH550 (γ aminopropyl Ethoxysilane) of 0.1g, continues
Stirring reaction 1.5h, still aging 12h, obtain milky alkaline silica sol color fixing agent.
The viscosity of this alkaline silica sol color fixing agent is 25mPa S, and solid content is 12%, silicon dioxide in alkaline silica sol color fixing agent
Mean particle size is 18.5nm.
Above example 1 is only the preferred embodiment of the invention, and in the present invention, alkaline silica sol color fixing agent can also be with positive silicon
Acetoacetic ester, water, alcohol, catalyst and silane coupler are raw material, are 1: 30～40: 20～30: 0.3～0.7 according to mol ratio:
After 0.001～0.01 mixes, prepared by sol gel reaction.Meanwhile, the condensing reflux temperature in step (3)
It it is 30 DEG C～60 DEG C；By the rate of addition that is added drop-wise in reactor of solution A of B solution and residue 70wt% be 1mL/min～
2mL/min；Stirring the response time be 0.5h～3h, speed of agitator is 400 turns/min～800 turns/min, digestion time be 8h～
12h；The mass percent concentration of ammonia is 25%～28% all can to implement, and the viscosity of the alkaline silica sol color fixing agent prepared can
Being distributed in 25mPa S～35mPa S, solid content is distributed in 10%～15%, silica dioxide granule average particle size distribution at 10nm～
20nm scope.
Embodiment 1 use silane coupler be γ aminopropyl Ethoxysilane, in the present invention, other silane coupler such as:
N-(β-aminoethyl)-γ-aminopropyl dimethoxy silane, VTES, vinyl-('beta '-methoxy ethyoxyl)
Silane；Or two or more mixture also can play and γ aminopropyl Ethoxysilane phase in these silane couplers
Same effect, and reach same or analogous technique effect.
Equally, embodiment 1 use alcoholic solvent be dehydrated alcohol, in the present invention, other alcoholic solvent such as: propanol, isopropyl
In alcohol, the tert-butyl alcohol, n-butyl alcohol or these alcoholic solvents, two or more mixture also can play identical with dehydrated alcohol
Effect, and reach same or analogous technique effect.
Embodiment 2:
Alkaline silica sol color fixing agent and the soda of embodiment 1 are contrasted, the investigation reactive dye colour fixation to wood staining:
Compound concentration is the activated red X-3B dye liquor of 1.0% (o.w.f), active red M-3BE dye liquor, reactive blue X-BR respectively
Dye liquor, reactive blue M-2GE dye liquor, reactive yellow X-R dye liquor, reactive yellow M-3RE dye liquor；It is separately added into 40g/L in each dye liquor
Matrii Sulfas Exsiccatus, with bath raio 1: 20,80 DEG C of constant temperature dyeing board using poplar board (specification 100 × 50 × 2mm) 3h.
Experimental group: add the alkaline silica sol color fixing agent of 8wt% (with dye liquor mass ratio) embodiment 1 gained in above-mentioned dye liquor,
Constant temperature fixation 80min at 60 DEG C, soaps, washes, is dried, obtain stained wood.
Matched group: add 20g/L soda color fixing agent, constant temperature fixation 80min at 60 DEG C in above-mentioned dye liquor, soap, wash,
It is dried, obtains stained wood.
Investigate the stained wood of alkaline silica sol fixation and soda fixation fastness to soaping (testing by GB/T3921-2008),
Resistance to dry, the data of wet friction color fastness (testing by GB/T 3920-2008), the results are shown in Table 1 in investigation.
Table 1: the colour fixation contrast table of alkaline silica sol color fixing agent and soda color fixing agent
Knowable to the comparing result of table 1, alkaline silica sol color fixing agent of the present invention is used to carry out the resistance to color of soaping of stained wood of fixation
Fastness reaches 4.5 grades, and the color fastness of resistance to dry friction reaches 4.5 grades, and moisture-proof colorfastness to rubbing reaches 4 grades, than traditional soda conduct
Stained wood that color fixing agent obtains is resistance to be soaped, the colorfastness to rubbing of resistance to dry and wet 3～4 grades want high 0.5～1 grade.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction.Although this
Invention discloses as above with preferred embodiment, but is not limited to the present invention.Any those of ordinary skill in the art,
In the case of the spirit of the present invention and technical scheme, all may utilize the method for the disclosure above and technology contents to this
Bright technical scheme makes many possible variations and modification, or is revised as the Equivalent embodiments of equivalent variations.Therefore, every do not take off
From the content of technical solution of the present invention, the technical spirit of the foundation present invention is to any simple modification made for any of the above embodiments, equivalent
Replace, equivalence changes and modifies, and all still falls within the range of technical solution of the present invention protection.
Claims (8)
1. an alkaline silica sol color fixing agent, it is characterized in that, described alkaline silica sol color fixing agent is with tetraethyl orthosilicate, water, alcohol, catalyst and silane coupler as raw material, according to mol ratio be 1: 30～40: 20～30: 0.3～0.7: 0.001～0.01 mix after, prepared by sol gel reaction；Described silane coupler is γ aminopropyl Ethoxysilane, N-(β-aminoethyl)-γ-aminopropyl dimethoxy silane, the mixture of one or more in VTES and vinyl-('beta '-methoxy ethyoxyl) silane.
Alkaline silica sol color fixing agent the most according to claim 1, it is characterised in that the viscosity of described alkaline silica sol color fixing agent is 25mPa s～35mPa s, solid content is 10%～15%, and silica dioxide granule mean diameter is 10nm～20nm.
3. the preparation method of alkaline silica sol color fixing agent described in a claim 1 or 2, it is characterised in that comprise the following steps:
(1) tetraethyl orthosilicate and alcoholic solvent are mixed, stir, be made into solution A；
(2) water is mixed homogeneously with catalyst, be made into B solution；
(3) take during described in 30wt%, solution A puts into reactor, it is warming up to 30 DEG C～60 DEG C, under agitation the solution A of described B solution and residue 70wt% is added drop-wise in reactor, with 30 DEG C～60 DEG C of condensing refluxes, after reaction 30min, then drip silane coupler, continue stirring reaction 0.5h～3h, ageing 8h～12h, completes the preparation of alkaline silica sol color fixing agent；Described silane coupler is γ aminopropyl Ethoxysilane, N-(β-aminoethyl)-γ-aminopropyl dimethoxy silane, the mixture of one or more in VTES and vinyl-('beta '-methoxy ethyoxyl) silane.
Preparation method the most according to claim 3, it is characterised in that the rate of addition solution A of B solution and residue 70wt% being added drop-wise in reactor in described step (3) is 1mL/min～2mL/min.
Preparation method the most according to claim 3, it is characterised in that in described step (3), mixing speed is 400 turns/min～800 turns/min.
6. according to the preparation method according to any one of claim 3 to 5, it is characterised in that described alcoholic solvent is the mixture of one or more in dehydrated alcohol, propanol, isopropanol, the tert-butyl alcohol and n-butyl alcohol.
7. according to the preparation method according to any one of claim 3 to 5, it is characterised in that described catalyst is ammonia.
Preparation method the most according to claim 7, it is characterised in that the mass percent concentration of described ammonia is 25%～28%.
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| CN105484072A (en) * | 2016-01-08 | 2016-04-13 | 湖州市千金丝织厂 | Novel alkaline silica sol color-fixing agent and preparation method thereof |
| CN108642923A (en) * | 2018-05-07 | 2018-10-12 | 合肥云都棉花有限公司 | A kind of garment material color fixing agent and preparation method thereof |
| CN109054507B (en) * | 2018-07-20 | 2022-07-19 | 中南林业科技大学 | Alkaline titanium sol color fixing agent and preparation method and application thereof |
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| CN101456201A (en) * | 2007-12-13 | 2009-06-17 | 章浩龙 | Treatment method of wood material |
| CN102345231B (en) * | 2011-07-13 | 2013-12-11 | 东华大学 | Silica nanoscale hybridized sol thermochromatic finishing method for fabric |
| CN103410007B (en) * | 2013-08-07 | 2016-01-06 | 东华大学 | A kind of sol-gel pH variable color method for sorting of textiles |
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