Summary of the invention
The technical problems to be solved by the present invention are: for traditional fluxing agent during hot dip, and in galvanizing flux containing aluminium
Aluminium generate the aluminium chloride that easily distils at a lower temperature, cause production scene to generate a large amount of harmful vapors, influence worker operation
And the problem of ambient enviroment, provide a kind of dedicated fluxing agent of galvanizing flux containing aluminium.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The dedicated fluxing agent of a kind of galvanizing flux containing aluminium, it is characterised in that: be made of the raw material of following parts by weight: 15~20
Part plant ash extract filter residue, 3~5 parts of calcinings material, 3~5 parts of calcirm-fluoride, 2~4 parts of emulsifier op-10s, 0.4~0.6 part is spat
Temperature -60,80~100 parts of dopamine solutions, 30~40 parts of water;
It is specific the preparation method is as follows:
(1) extraction of plant ash extract filter residue: by crystallisation by cooling after plant ash and mixed in hydrochloric acid, filtering and concentration, then
Filtered and be drying to obtain plant ash extract filter residue;
(2) synthesis of calcining material:, with activated yeast mixture mixed fermentation, modified dacron will be obtained after polyester fiber dipping by lye
Short fibre, then the gained short fibre of modified dacron is added after citric acid is mixed with cerous nitrate solution, it is centrifugated after reaction, then washed
Expect with being calcined after drying to get calcining;
(3) preparation of fluxing agent: by plant ash extract filter residue, calcirm-fluoride, emulsifier op-10, Tween-60, dopamine
After solution and water are uniformly mixed, calcining material is added, continues to discharge after being stirred filling.
The dopamine solution mass concentration is 2g/L.
Concentration condition described in step (1) are as follows: in Rotary Evaporators, in temperature be 80~85 DEG C, pressure be 0.06~
Under the conditions of 0.08MPa, 30~45min of concentrated by rotary evaporation.
Crystallisation by cooling condition described in step (1) are as follows: temperature is 2~4 DEG C, and the time is 3~5h.
Polyester fiber diameter described in step (2) is 1.0~1.4mm.
The preparation steps of activated yeast mixture described in step (2) are as follows: by active dry yeast, pour into and be preheated to 33~35 DEG C of temperature
In water, 25~30min of stir-activating.
Calcination condition described in step (2) are as follows: be warming up to 780~800 DEG C with 3~5 DEG C/min rate program, heat preservation calcining
After 2~4h, room temperature is cooled to the furnace.
The present invention is compared with other methods, and advantageous effects are:
(1) the invention firstly uses hydrochloric acid reacts with plant ash, and main component is potassium carbonate in plant ash, in addition also contains
After phosphorus, potassium carbonate and phosphorus containing components are reacted with hydrochloric acid, generates corresponding metal hydrochloride and metal phosphate and is dissolved in water,
It is concentrated after crystallisation by cooling, reduce water in solubility salt solubility and make its crystallization be precipitated, the metal hydrochloride of precipitation and
Phosphate is as principle active component in plant ash extract filter residue, in use, reactive aluminum in phosphate and fluxing agent,
Aluminum phosphate is generated, the molten boiling point of the aluminum phosphate of generation is higher for aluminium chloride, can be by aluminium chloride fixed packet in part in system
It covers, avoids aluminum chloride sublimation at a lower temperature and production scene is caused to have a large amount of harmful vapors;
(2) present invention utilizes alkali liquid corrosion polyester fiber, so that PET fiber surface is formed pit, then mix and send out with saccharomycete
Ferment makes saccharomycete fixed growth in polyester fiber pit, consumes citric acid followed by saccharomycete tricarboxylic acid cycle, makes solution
The cerium ion of middle complexing discharges, at the same the carbon dioxide that generates of saccharomycete aerobic respiration make in saccharomycete surrounding medium carbonate from
Sub- concentration is promoted, and is formed carbonic acid cerium crystal in conjunction with cerium ion, and adsorbed by the organic matter on saccharomycete surface, is washed to be fixed on
In synthetic fibre fiber pit, carbonic acid cerium crystal further long macro aggregate is avoided, then the other cerium oxide of ultrafine nanometer is made through calcining,
The effect for improving the current efficiency of electroplate liquid, while the filming performance for cooperating dopamine solution excellent, suppression can be played in fluxing agent
The generation of aluminium chloride processed, solves the problems, such as aluminum chloride sublimation from source.
Specific embodiment
300~500g plant ash is weighed first, pours into the beaker for filling that 800~1000mL mass fraction is 8~10% hydrochloric acid
In, then beaker immigration digital display tested the speed constant temperature blender with magnetic force, it is 75~85 DEG C in temperature, revolving speed is 300~500r/min item
Under part, constant temperature is stirred 20~40min, then by material filtering in beaker, obtains filtrate, and gained filtrate is transferred to rotary evaporation
Instrument is 80~85 DEG C in temperature, and under the conditions of pressure is 0.06~0.08MPa, 30~45min of concentrated by rotary evaporation obtains concentrate;By institute
It obtains concentrate to be transferred in refrigerator, refrigerates 3~5h under the conditions of being 2~4 DEG C in temperature, then the concentrate after refrigeration is filtered, must filter
Slag, and gained filter residue is transferred in baking oven, it dries under the conditions of being 105~110 DEG C in temperature to constant weight, obtains the filter of plant ash extract
Slag;The polyester fiber that 200~300g diameter is 1.0~1.4mm is weighed again, and being cut into length is 2~4cm terylene short fiber, and will
Gained terylene short fiber, which pours into, to be filled in the beaker that 500~700mL mass fraction is 10~15% sodium hydroxide solutions, and glass bar is used
After being stirred 10~20min, be standing and soaking 3~5h, then by material filtering in beaker, and be washed with deionized filter cake until
Cleaning solution is in neutrality, and obtains pretreatment terylene short fiber;Gained pretreatment terylene short fiber is poured into and fills 800~1000mL self-control liquid
In the fermentor of culture medium, and 80~100mL activated yeast mixture is added into fermentor, is stirred with the glass bar after disinfection
After 10~20min, fermentor is sealed, under the conditions of temperature is 28~30 DEG C, 10~12h of constant-temperature enclosed fermentation, then will fermentation
Material filtering in tank obtains the short fibre of modified dacron;Weigh 20~30g citric acid, pour into fill 400~600mL mass fraction be 6~
In the three-necked flask of 8% cerous nitrate solution, after being stirred 20~30min with glass bar, 80~100g is added into three-necked flask
The short fibre of gained modified dacron, then three-necked flask is moved into water-bath, under the conditions of temperature is 28~30 DEG C, with 3~5mL/min
Rate material into three-necked flask is passed through air, is continually fed into after 3~5h material in three-necked flask being transferred to centrifuge, with 6800
~7000r/min revolving speed is centrifugated 10~15min, discards upper liquid, obtains lower sediment thing;Gained lower sediment thing is spent
Ion water washing 3~5 times, then the lower sediment thing after washing is transferred in baking oven, it is done under the conditions of being 105~110 DEG C in temperature
It is dry and the lower sediment thing after drying to be transferred to Muffle furnace to constant weight, 780~800 are warming up to 3~5 DEG C/min rate program
DEG C, after 2~4h of heat preservation calcining, cools to room temperature with the furnace, discharge, material must be calcined;According to parts by weight, successively add in batch mixer
Enter 3~5 parts of gained calcinings to expect, 3~5 parts of calcirm-fluoride, 2~4 parts of emulsifier op-10s, 0.4~0.6 part of Tween-60,15~20 parts
Plant ash extract filter residue, 80~100 parts of mass concentrations are 2g/L dopamine solution, and 30~40 parts of deionized waters are in temperature
45~55 DEG C, under the conditions of revolving speed is 600~800r/min, after constant temperature is stirred 2~4h, cooled to room temperature, discharging, i.e.,
The dedicated fluxing agent of aluminium galvanizing flux must be contained.Wherein self-control fluid nutrient medium be by 10~20g sucrose, 8~10g glucose, 0.3~
0.5g potassium dihydrogen phosphate, 0.1~0.2g magnesium chloride, 0.1~0.2g calcium chloride, 0.2~0.4g ferrous sulfate, 8~10mL grape
Juice is mixed with 1000~1200mL deionized water.The concrete configuration step of activated yeast mixture are as follows: weigh the dry ferment of 4~8g activity
Mother pours into and fills 100~150mL and be preheated in the beaker of 33~35 DEG C of warm water, with glass bar 25~30min of stir-activating, obtains
Activated yeast mixture.
Example 1
500g plant ash is weighed first, is poured into and is filled in the beaker that 1000mL mass fraction is 10% hydrochloric acid, then beaker is moved
Entering digital display to test the speed constant temperature blender with magnetic force, is 85 DEG C in temperature, under the conditions of revolving speed is 500r/min, constant temperature is stirred 40min,
Again by material filtering in beaker, filtrate is obtained, and gained filtrate is transferred to Rotary Evaporators, is 85 DEG C in temperature, pressure is
Under the conditions of 0.08MPa, concentrated by rotary evaporation 45min obtains concentrate;Gained concentrate is transferred in refrigerator, under the conditions of temperature is 4 DEG C
Refrigerate 5h, then by after refrigeration concentrate filter, obtain filter residue, and gained filter residue is transferred in baking oven, in temperature be 110 DEG C of conditions
Lower drying obtains plant ash extract filter residue to constant weight;The polyester fiber that 300g diameter is 1.4mm is weighed again, and being cut into length is
4cm terylene short fiber, and gained terylene short fiber is poured into and is filled in the beaker that 700mL mass fraction is 15% sodium hydroxide solution, it uses
After glass bar is stirred 20min, be standing and soaking 5h, then by material filtering in beaker, and be washed with deionized filter cake until
Cleaning solution is in neutrality, and obtains pretreatment terylene short fiber;Gained pretreatment terylene short fiber is poured into and fills 1000mL self-control Liquid Culture
In the fermentor of base, and 100mL activated yeast mixture is added into fermentor, after being stirred 20min with the glass bar after disinfection,
Fermentor is sealed, under the conditions of temperature is 30 DEG C, constant-temperature enclosed fermentation 12h, then by material filtering in fermentor, obtain Modified Polyester
The short fibre of synthetic fibre;30g citric acid is weighed, pours into and fills in the three-necked flask that 600mL mass fraction is 8% cerous nitrate solution, use glass bar
After being stirred 30min, the short fibre of modified dacron obtained by 100g is added into three-necked flask, then three-necked flask is moved into water-bath
In, under the conditions of temperature is 30 DEG C, with 5mL/min rate, into three-necked flask, material is passed through air, is continually fed into three after 5h
Material is transferred to centrifuge in mouth flask, is centrifugated 15min with 7000r/min revolving speed, discards upper liquid, obtain lower sediment thing;
Gained lower sediment thing is washed with deionized 5 times, then the lower sediment thing after washing is transferred in baking oven, is in temperature
It dries under the conditions of 110 DEG C to constant weight, and the lower sediment thing after drying is transferred to Muffle furnace, with the heating of 5 DEG C/min rate program
To 800 DEG C, after heat preservation calcining 4h, cools to room temperature with the furnace, discharge, material must be calcined;According to parts by weight, in batch mixer successively
5 parts of gained calcinings are added to expect, 5 parts of calcirm-fluoride, 4 parts of emulsifier op-10s, 0.6 part of Tween-60,20 parts of plant ash extract filter residues,
100 parts of mass concentrations are 2g/L dopamine solution, 40 parts of deionized waters, in temperature be 55 DEG C, under the conditions of revolving speed is 800r/min,
After constant temperature is stirred 4h, cooled to room temperature discharges to get the dedicated fluxing agent of galvanizing flux containing aluminium.Wherein self-control liquid training
Feeding base be by 20g sucrose, 10g glucose, 0.5g potassium dihydrogen phosphate, 0.2g magnesium chloride, 0.2g calcium chloride, 0.4g ferrous sulfate,
10mL grape juice is mixed with 1200mL deionized water.The concrete configuration step of activated yeast mixture are as follows: weigh the dry ferment of 8g activity
Mother pours into and fills 150mL and be preheated in the beaker of 35 DEG C of warm water, with glass bar stir-activating 30min, obtains activated yeast mixture.
Example 2
300g plant ash is weighed first, is poured into and is filled in the beaker that 800mL mass fraction is 8% hydrochloric acid, then beaker is moved into
Digital display tests the speed constant temperature blender with magnetic force, is 75 DEG C in temperature, and under the conditions of revolving speed is 300r/min, constant temperature is stirred 20min, then
By material filtering in beaker, obtain filtrate, and gained filtrate be transferred to Rotary Evaporators, in temperature be 80 DEG C, pressure 0.06MPa
Under the conditions of, concentrated by rotary evaporation 30min obtains concentrate;Gained concentrate is transferred in refrigerator, refrigerates 3h under the conditions of being 2 DEG C in temperature,
The concentrate after refrigeration is filtered again, obtains filter residue, and gained filter residue is transferred in baking oven, it is dry under the conditions of being 105 DEG C in temperature
To constant weight, plant ash extract filter residue is obtained;The polyester fiber that 200g diameter is 1.0mm is weighed again, and being cut into length is 2cm terylene
Short fibre, and gained terylene short fiber is poured into and is filled in the beaker that 500mL mass fraction is 10% sodium hydroxide solution, use glass bar
After being stirred 10min, it is standing and soaking 3h, then by material filtering in beaker, and filter cake is washed with deionized until cleaning solution
It is in neutrality, obtains pretreatment terylene short fiber;Gained pretreatment terylene short fiber is poured into the fermentation for filling 800mL self-control fluid nutrient medium
In tank, and 80mL activated yeast mixture is added into fermentor, after being stirred 10min with the glass bar after disinfection, by fermentor
Sealing, under the conditions of temperature is 28 DEG C, constant-temperature enclosed fermentation 10h, then by material filtering in fermentor, obtain the short fibre of modified dacron;
20g citric acid is weighed, pours into and fills in the three-necked flask that 400mL mass fraction is 6% cerous nitrate solution, is stirred with glass bar mixed
After closing 20min, the short fibre of modified dacron obtained by 80g is added into three-necked flask, then three-necked flask is moved into water-bath, in temperature
Under the conditions of 28 DEG C, with 3mL/min rate, into three-necked flask, material is passed through air, is continually fed into object in three-necked flask after 3h
Material is transferred to centrifuge, is centrifugated 10min with 6800r/min revolving speed, discards upper liquid, obtain lower sediment thing;By gained lower layer
Sediment is washed with deionized 3 times, then the lower sediment thing after washing is transferred in baking oven, under the conditions of temperature is 105 DEG C
It dries to constant weight, and the lower sediment thing after drying is transferred to Muffle furnace, be warming up to 780 DEG C with 3 DEG C/min rate program, heat preservation
After calcining 2h, room temperature is cooled to the furnace, discharge, must calcine material;According to parts by weight, 3 parts of gained are sequentially added in batch mixer
Calcining material, 3 parts of calcirm-fluoride, 2 parts of emulsifier op-10s, 0.4 part of Tween-60,15 parts of plant ash extract filter residues, 80 parts of quality are dense
Degree is 2g/L dopamine solution, and 30 parts of deionized waters are 45 DEG C in temperature, and under the conditions of revolving speed is 600r/min, constant temperature stirring is mixed
After closing 2h, cooled to room temperature discharges to get the dedicated fluxing agent of galvanizing flux containing aluminium.Wherein self-control fluid nutrient medium be by:
10g sucrose, 8g glucose, 0.3g potassium dihydrogen phosphate, 0.1g magnesium chloride, 0.1g calcium chloride, 0.2g ferrous sulfate, 8mL grape juice
It is mixed with 1000mL deionized water.The concrete configuration step of activated yeast mixture are as follows: weigh 4g active dry yeast, pour into and fill
100mL is preheated in the beaker of 33 DEG C of warm water, with glass bar stir-activating 25min, obtains activated yeast mixture.
Example 3
400g plant ash is weighed first, is poured into and is filled in the beaker that 900mL mass fraction is 9% hydrochloric acid, then beaker is moved into
Digital display tests the speed constant temperature blender with magnetic force, is 80 DEG C in temperature, and under the conditions of revolving speed is 400r/min, constant temperature is stirred 30min, then
By material filtering in beaker, obtain filtrate, and gained filtrate be transferred to Rotary Evaporators, in temperature be 82 DEG C, pressure 0.07MPa
Under the conditions of, concentrated by rotary evaporation 35min obtains concentrate;Gained concentrate is transferred in refrigerator, refrigerates 4h under the conditions of being 3 DEG C in temperature,
The concentrate after refrigeration is filtered again, obtains filter residue, and gained filter residue is transferred in baking oven, it is dry under the conditions of being 107 DEG C in temperature
To constant weight, plant ash extract filter residue is obtained;The polyester fiber that 250g diameter is 1.2mm is weighed again, and being cut into length is 3cm terylene
Short fibre, and gained terylene short fiber is poured into and is filled in the beaker that 600mL mass fraction is 12% sodium hydroxide solution, use glass bar
After being stirred 15min, it is standing and soaking 4h, then by material filtering in beaker, and filter cake is washed with deionized until cleaning solution
It is in neutrality, obtains pretreatment terylene short fiber;Gained pretreatment terylene short fiber is poured into the fermentation for filling 900mL self-control fluid nutrient medium
In tank, and 90mL activated yeast mixture is added into fermentor, after being stirred 15min with the glass bar after disinfection, by fermentor
Sealing, under the conditions of temperature is 29 DEG C, constant-temperature enclosed fermentation 11h, then by material filtering in fermentor, obtain the short fibre of modified dacron;
25g citric acid is weighed, pours into and fills in the three-necked flask that 500mL mass fraction is 7% cerous nitrate solution, is stirred with glass bar mixed
After closing 25min, the short fibre of modified dacron obtained by 90g is added into three-necked flask, then three-necked flask is moved into water-bath, in temperature
Under the conditions of 29 DEG C, with 4mL/min rate, into three-necked flask, material is passed through air, is continually fed into object in three-necked flask after 4h
Material is transferred to centrifuge, is centrifugated 13min with 6900r/min revolving speed, discards upper liquid, obtain lower sediment thing;By gained lower layer
Sediment is washed with deionized 4 times, then the lower sediment thing after washing is transferred in baking oven, under the conditions of temperature is 107 DEG C
It dries to constant weight, and the lower sediment thing after drying is transferred to Muffle furnace, be warming up to 790 DEG C with 4 DEG C/min rate program, heat preservation
After calcining 3h, room temperature is cooled to the furnace, discharge, must calcine material;According to parts by weight, 4 parts of gained are sequentially added in batch mixer
Calcining material, 4 parts of calcirm-fluoride, 3 parts of emulsifier op-10s, 0.5 part of Tween-60,17 parts of plant ash extract filter residues, 90 parts of quality are dense
Degree is 2g/L dopamine solution, and 35 parts of deionized waters are 47 DEG C in temperature, and under the conditions of revolving speed is 700r/min, constant temperature stirring is mixed
After closing 3h, cooled to room temperature discharges to get the dedicated fluxing agent of galvanizing flux containing aluminium.Wherein self-control fluid nutrient medium be by:
15g sucrose, 9g glucose, 0.4g potassium dihydrogen phosphate, 0.1g magnesium chloride, 0.1g calcium chloride, 0.3g ferrous sulfate, 9mL grape juice
It is mixed with 1100mL deionized water.The concrete configuration step of activated yeast mixture are as follows: weigh 7g active dry yeast, pour into and fill
120mL is preheated in the beaker of 34 DEG C of warm water, with glass bar stir-activating 27min, obtains activated yeast mixture.
Reference examples: zinc ammonium chloride
Select quality 500g, surface area 0.06m2Steel workpiece, and four steel workpiece surfaces are cleaned, guarantee steel
Material workpiece surface is clean, then respectively by the steel workpiece after this four cleanings be placed in example 1 that temperature is 65 DEG C to example 3 and
In the fluxing agent of reference examples, 3min is impregnated, takes out the steel test specimen after helping plating, and the iron and steel parts after plating will be helped in 120 DEG C of items
It under part after dry 22min, moves in galvanizing flux containing aluminium, is to carry out hot galvanizing 2min at 460 DEG C in temperature, steel examination can be completed
Part it is zinc-plated.
Apparent mass detection, testing result such as table 1 are carried out to the steel workpiece after zinc-plated.
Table 1
Example |
Brightness |
Whether there is or not plating leakages |
There is non smoke |
Example 1 |
It is bright |
Nothing |
Nothing |
Example 2 |
It is bright |
Nothing |
Nothing |
Example 3 |
It is bright |
Nothing |
Nothing |
Reference examples |
It is rougher |
Have, but seldom |
On a small quantity |
As can be seen from Table 1, fluxing agent prepared by the present invention helps plating effect good, helps apparent mass after plating good.
Four steel test specimens after zinc-plated are placed in YWXQ/750 type salt spray test chamber, by GB/T10125-1997 " people
Gas making atmosphere corrosion test salt spray test " it is executed, is continuously detected after 720h by spraying, utilize formula V=(W1-W2)/
(St), wherein W1For the steel product quality before corrosion, W2For the steel product quality after corrosion, S is surface area, and t is spray time, inspection
It surveys and calculates data such as table 2:
Table 2
Example |
W1(g) |
W2(g) |
S(m2) |
T(h) |
V(g/(m2H)) |
Example 1 |
500 |
495.68 |
0.06 |
720 |
0.1 |
Example 2 |
500 |
493.52 |
0.06 |
720 |
0.15 |
Example 3 |
500 |
491.36 |
0.06 |
720 |
0.20 |
Reference examples |
500 |
487.04 |
0.06 |
720 |
0.3 |
As can be seen from Table 2, fluxing agent prepared by the present invention Corrosion Protection with higher.