A kind of preparation method of nickel plating solution detin adsorbent
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the preparation side of particularly a kind of nickel plating solution detin adsorbent
Method.
Background technology
The fault being commonly encountered in nickel plating solution, such as: pin hole, pit, decortication, coarse, turn black, grow dim, striped and embrittlement etc.,
Except minority is owing to solution composition imbalance, operating condition exceed technological specification in addition to causing, often miscellaneous with plating solution
Matter is relevant.Tin impurity is more sensitive to nickel plating solution, when concentration reaches certain value, may result in the low current density district of plating piece
Coating turns black.In the case that metallic nickel price escalates, some enterprises before workpiece barrel plating bright nickel, first plate in tin copper
Ashbury metal, then plates one layer of thin nickel again, thus reduces the purpose of electroplating cost.According to this procedure operation, a small amount of copper
Carried people's nickel bath with tin impurity.The current potential calibration of copper, can deposit in coating quickly.Stannous ion can be with nickel plating light
Some composition of bright dose and catabolite thereof generate complex compound, and electrode potential is more negative in addition, and electrodeposition rate is relatively slow, therefore, sub-
Tin ion can retain the long period affects the performance of plating solution in the plating solution.
CN101956074A discloses a kind of method removing tin from zinc aqueous slkali, relates to a kind of alkali leaching-electrolysis raw
Pan belongs to the removal technology of tin in Zinc powder process leachate.First it is Sn by Theil indices > the zinc aqueous slkali of 2~7g/L is heated to 70
~100 DEG C, then under the conditions of stirring (200~700r/min), adding metal zinc (100~400 mesh), metal zinc presses zinc
In aqueous slkali, 3~12 times (i.e. Zn: Sn=3~12: 1 mol ratios) of tin molar content add, and react 3~15h, stop stirring, take advantage of
Heat filtering, in the filtrate that detection is filtrated to get, tin concentration is less than 0.05g/L, and direct power transmission is long-pending carries zinc, and filter residue is for containing 90~95%
Thick tin, sells.The present invention has except advantages such as tin are thorough, method is easy, can eliminate tin to follow-up Zinc electrolysis by the present invention
The serious harm that process causes, ensures that Zinc electrolysis process is smoothed out, also can obtain the thick tin by-product with high added value simultaneously
Product.
CN105217759A discloses a kind of waste water and removes tin agent except tin agent and preparation method thereof, above-mentioned waste water, by comprising
The component of following weight portion is made: alundum (Al2O3) 15-20 part, calcium aluminate 8-11 part, diatomite 5-8 part, basic magnesium carbonate 4-7
Part, ferrous sulfate 2-4 part, polyethylene 2-3 part, potassium fluorozirconate 2-4 part, borosilicic acid 1-3 part, hydroxypropul starch sodium phosphate 2-3 part
With dimethyl diallyl ammonium chloride 1-2 part.Present invention also offers a kind of waste water except the preparation method of tin agent.
The method removing tin impurity reported in current document, complicated component, easily entrain new impurity, so needing to send out
Bright a kind of novel sorbing material, improves the adsorption capacity to tin.
Content of the invention
For the deficiencies in the prior art, the invention provides the preparation method of a kind of nickel plating solution detin adsorbent.By hydroxyl
Propyl group dextran microspheres carries out amination, adds (dimethyl amine) tin trimethyl, and double lauryl amines are aminating agent, can prepare absorption
Agent.
The preparation method of a kind of nickel plating solution detin adsorbent, comprises the following steps:
Hydroxypropyl dextran microspheres methyl alcohol is made sweller, and consumption is the 200-500% of hydroxypropyl dextran microspheres weight
(wt);At a temperature of 20-50 DEG C, adding the reaction of (dimethyl amine) tin trimethyl, consumption is hydroxypropyl dextran microspheres weight
1-10% (wt), add double lauryl amine, be the 100-200% (wt) of hydroxypropyl dextran microspheres weight, be incubated 5-15h,
The adsorbent being applied to remove tin ion can be prepared.
Described hydroxypropyl dextran microspheres can use commercially available prod, as Xi'an Sunresin New Materials Co., Ltd. is raw
The hydroxypropyl dextran microspheres product producing.
Described (dimethyl amine) tin trimethyl, double lauryl amines can use commercially available prod.
Beneficial effects of the present invention:
The present invention uses hydroxypropyl dextran microspheres with aldehyde functions, through (dimethyl amine) tin trimethyl, double dodecanes
Base amine amination generates dextran amine, introduces tin element, can improve the absorption property to tin impurity, nickel plating solution on microballoon skeleton
In tin ion concentration be smaller than 1mg/L.
Detailed description of the invention
Following example only further illustrate the present invention, are not to limit the scope of protection of the invention.
Embodiment 1
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 300Kg methyl alcohol;At a temperature of 30 DEG C, add
(dimethyl amine) tin trimethyl reacts, and consumption is 5Kg, adds the double lauryl amine of 150Kg, is incubated 8h, filters, dry numbering
For SX-1.
Embodiment 2
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 200Kg methyl alcohol;At a temperature of 20 DEG C, add
(dimethyl amine) tin trimethyl reacts, and consumption is 1Kg, adds the double lauryl amine of 100Kg, is incubated 5h, filters, dry, product
Numbered SX-2.
Embodiment 3
In 1000L reactor, add 100Kg hydroxypropyl dextran microspheres, add 500Kg methyl alcohol;At a temperature of 50 DEG C, add
(dimethyl amine) tin trimethyl reacts, and consumption is 10Kg, adds 20Kg ferric trichloride, adds the double lauryl amine of 200Kg, insulation
15h, filters, and dries, and production code member is SX-3.
Comparative example 1
It is added without (dimethyl amine) tin trimethyl, the other the same as in Example 1.The numbered SX-4 of products obtained therefrom.
Comparative example 2
It is added without double lauryl amine, the other the same as in Example 1.The numbered SX-5 of products obtained therefrom.
Comparative example 3
It is added without double lauryl amine, (dimethyl amine) tin trimethyl, the other the same as in Example 1.The numbered SX-6 of products obtained therefrom.
Embodiment 4
Prepare nickel plating solution with AR: six hydration nickel sulfate 200g/L, Nickel dichloride hexahydrate 50 g/L, boric acid 45g/L,
Regulate plating solution pH=4.7 with sodium carbonate liquor, backward plating solution adds stannous chloride, makes the mass concentration of stannous ion reach
150mg/L。
Accurately weigh each 5g of adsorbent that pretreated embodiment 1-3 and comparative example 1-3 prepare, be placed in 250mL tool plug
In ground triangular flask, precision adds the nickel plating solution that people 100mL configures, and triangular flask at room temperature vibrates 5h, fully adsorbs
After, to filter, detection calculates the tin ion concentration after absorption in nickel plating solution, is shown in Table 1:
Table 1: list after the separation material absorption that this patent prepares
Production code member |
Tin ion concentration mg/L in nickel plating solution after absorption |
W-1 |
0.9 |
W-2 |
1.1 |
W-3 |
0.7 |
W-4 |
3.6 |
W-5 |
4.9 |
W-6 |
18.2 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.It any with the present invention is
Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent replaces
Change or modification etc., be all covered by among protection scope of the present invention.