Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, the ion sieve that provide that a kind of adsorption capacity is higher, adsorption rate comparatively fast and can stripping have dysgenic removal aflatoxin to health.
Second purpose of the present invention provides a kind of preparation method who removes the ion sieve of aflatoxin.
A kind of ion sieve of removing aflatoxin, make with following method:
(1) ratio in mass ratio 1:30-50 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 8-16 hour;
(2) ratio in mass ratio 1:10-50 adds the phenyl trimethylammonium bromide in the deionized water, at 60-120r/min, stirs 1-100min, filters, and gets clear filtrate, and is standby;
(3) in the ratio of mass ratio 1:60-100, CuCl is added in the ammoniacal liquor that mass concentration is 18%-30%, stir 10-30min, filter to get filtrate at 60-100r/min, standby;
(4) keeping mixing speed 60-120r/min, pH is 7-9, and under the temperature 25-60 ℃ of condition, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 5-10 hour;
(5) after the even gel that step (4) is obtained removes free water, with deionized water solable matter in the filter cake is cleaned, again with gained solid vacuum freeze drying, maintain the temperature at-10 ℃ to 0 ℃ after the freeze-drying, be incubated 1-3 hour, grinding is sieved, and gets the ion sieve that graininess is removed aflatoxins.
Preferably step (1) is: the ratio in mass ratio 1:40 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 12 hours.
Step (2) is: the ratio in mass ratio 1:30 adds the phenyl trimethylammonium bromide in the deionized water, at 80r/min, stirs 50min, filters, and gets clear filtrate, and is standby.
Step (3) is: in the ratio of mass ratio 1:80, it is in 25% the ammoniacal liquor that CuCl is added mass concentration, stirs 20min at 80r/min, filters to get filtrate, standby.
Step (4) is: keeping mixing speed 80r/min, pH is 8, and under 40 ℃ of conditions of temperature, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 8 hours.
A kind of preparation method who removes the ion sieve of aflatoxin, be made up of following step:
(1) ratio in mass ratio 1:30-50 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 8-16 hour;
(2) ratio in mass ratio 1:10-50 adds the phenyl trimethylammonium bromide in the deionized water, at 60-120r/min, stirs 1-100min, filters, and gets clear filtrate, and is standby;
(3) in the ratio of mass ratio 1:60-100, CuCl is added in the ammoniacal liquor that mass concentration is 18%-30%, stir 10-30min, filter to get filtrate at 60-100r/min, standby;
(4) keeping mixing speed 60-120r/min, pH is 7-9, and under the temperature 25-60 ℃ of condition, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 5-10 hour;
(5) after the even gel that step (4) is obtained removes free water, with deionized water solable matter in the filter cake is cleaned, again with gained solid vacuum freeze drying, maintain the temperature at-10 ℃ to 0 ℃ after the freeze-drying, be incubated 1-3 hour, grinding is sieved, and gets the ion sieve that graininess is removed aflatoxins.
Preferably step (1) is: the ratio in mass ratio 1:40 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 12 hours.
Step (2) is: the ratio in mass ratio 1:30 adds the phenyl trimethylammonium bromide in the deionized water, at 80r/min, stirs 50min, filters, and gets clear filtrate, and is standby.
Step (3) is: in the ratio of mass ratio 1:80, it is in 25% the ammoniacal liquor that CuCl is added mass concentration, stirs 20min at 80r/min, filters to get filtrate, standby.
Step (4) is: keeping mixing speed 80r/min, pH is 8, and under 40 ℃ of conditions of temperature, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 8 hours.
A kind of ion sieve of removing aflatoxin of the present invention is fast to the aflatoxins adsorption rate, the adsorption capacity height.When being used to handle aflatoxins content and being higher than the food of 10 μ g/kg, guaranteeing out that aflatoxins content is lower than under the prerequisite of 2.0 μ g/kg, average adsorption capacity can reach 390 μ gAFB/g and can stripping to health dysgenic material do not arranged greater than general adsorbent.Method of the present invention is simple.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of ion sieve of removing aflatoxin, make with following method:
(1) at 25 ℃-30 ℃, in the beaker of 1000mL, add 10g sodium-based montmorillonite (MMT) and 490ml deionized water, 60r/min stirs, and leaves standstill 12 hours, and fully swelling forms suspension;
(2) take by weighing 6.4836g phenyl trimethylammonium bromide (PTMAB) in addition and be dissolved in the 100mL deionized water,, stir 10min, filter, get clear filtrate with triangular funnel at 80r/min, standby;
(3) taking by weighing 1.08g CuCl, to be dissolved in the 100mL mass concentration be in 25% the ammoniacal liquor, stirs 20min at 80r/min, filters to get filtrate, standby;
(4) then under the stirring condition of 60r/min, pH is 8, under 40 ℃ of conditions of temperature, with PTMAB solution and CuCl ammonia spirit respectively at continuing evenly to add in the suspension that step (1) makes with the speed of 2.0ml/min in the separatory funnel, the sample that obtains when finishing is white pulpous state system, the particle diameter that wherein evenly is scattered here and there is the gel particle of 2-7mm, after the ageing 5 hours, suction filtration, spend deionised water chloride ion content to the wash water and with the freeze-drying after freezing 12 hours of gained solid, maintain the temperature at 0 ℃ after the freeze-drying less than 10mg/L, be incubated 2 hours, ground 120 mesh sieves and promptly get the ion sieve that graininess is removed aflatoxins.This finished product is used to handle the aqueous solution that aflatoxins content is 1.0ppm, is guaranteeing that water outlet aflatoxins content is lower than under the prerequisite of 5.0ppb, and average adsorbance is the 396ugAFB/g ion sieve.
Embodiment 2
(1) at 25 ℃-30 ℃, in the beaker of 1000mL, add 5g sodium-based montmorillonite (MMT) and 200ml ionized water, 50r/min stirs, and leaves standstill 12 hours, and fully swelling forms suspension;
(2) take by weighing 2.23g phenyl trimethylammonium bromide (PTMAB) in addition and be dissolved in the 60mL deionized water,, stir 10min, filter, get clear filtrate with triangular funnel at 80r/min, standby;
(3) taking by weighing 0.55g CuCl, to be dissolved in the 60mL mass concentration be in 25% the ammoniacal liquor, stirs 20min at 80r/min, filters to get filtrate, standby;
(4) then under the stirring condition of 50r/min, pH is 8, under 40 ℃ of conditions of temperature, with PTMAB solution and CuCl ammonia spirit respectively at continuing evenly to add in the suspension that step (1) makes with the speed of 10ml/min in the separatory funnel, the sample that obtains when finishing is white pulpous state system, the particle diameter that wherein evenly is scattered here and there is the gel particle of 2-7mm, after the ageing 6 hours, suction filtration, spend deionised water chloride ion content to the wash water and with the freeze-drying after freezing 12 hours of gained solid, maintain the temperature at 0 ℃ after the freeze-drying less than 10mg/L, be incubated 2 hours, ground 120 mesh sieves and promptly get the ion sieve that graininess is removed aflatoxins.This finished product is used to handle the aqueous solution that aflatoxins content is 1.0ppm, is guaranteeing that water outlet aflatoxins content is lower than under the prerequisite of 5.0ppb, and average adsorbance is the 394.5ug/g ion sieve.
Embodiment 3
A kind of ion sieve of removing aflatoxin, make with following method:
(1) ratio in mass ratio 1:30 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 8 hours;
(2) ratio in mass ratio 1:10 adds the phenyl trimethylammonium bromide in the deionized water, at 120r/min, stirs 1min, filters, and gets clear filtrate, and is standby;
(3) in the ratio of mass ratio 1:60, it is in 30% the ammoniacal liquor that CuCl is added mass concentration, stirs 20min at 80r/min, filters to get filtrate, standby;
(4) keeping mixing speed 120r/min, pH is 8, and under 60 ℃ of conditions of temperature, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 10 hours;
(5) after the even gel that step (4) is obtained removes free water, with deionized water solable matter in the filter cake is cleaned, again with gained solid vacuum freeze drying, maintain the temperature at-10 ℃ after the freeze-drying, be incubated 3 hours, grinding is sieved, and gets the ion sieve that graininess is removed aflatoxins.
Embodiment 4
A kind of ion sieve of removing aflatoxin, make with following method:
(1) ratio in mass ratio 1:50 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 16 hours;
(2) ratio in mass ratio 1:50 adds the phenyl trimethylammonium bromide in the deionized water, at 60r/min, stirs 100min, filters, and gets clear filtrate, and is standby;
(3) in the ratio of mass ratio 1:100, it is in 18% the ammoniacal liquor that CuCl is added mass concentration, stirs 30min at 60r/min, filters to get filtrate, standby;
(4) keeping mixing speed 60r/min, pH is 7, and under 25 ℃ of conditions of temperature, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 5 hours;
(5) after the even gel that step (4) is obtained removes free water, with deionized water solable matter in the filter cake is cleaned, again with gained solid vacuum freeze drying, maintain the temperature at 0 ℃ after the freeze-drying, be incubated 1 hour, grinding is sieved, and gets the ion sieve that graininess is removed aflatoxins.
Embodiment 5
A kind of ion sieve of removing aflatoxin, make with following method:
(1) ratio in mass ratio 1:40 adds sodium-based montmorillonite in the deionized water, soaks to become suspension in 12 hours;
(2) ratio in mass ratio 1:30 adds the phenyl trimethylammonium bromide in the deionized water, at 80r/min, stirs 50min, filters, and gets clear filtrate, and is standby;
(3) in the ratio of mass ratio 1:80, it is in 25% the ammoniacal liquor that CuCl is added mass concentration, stirs 10min at 100r/min, filters to get filtrate, standby;
(4) keeping mixing speed 80r/min, pH is 9, and under 40 ℃ of conditions of temperature, the filtrate that step (2) and step (3) are made splashes in the suspension that step (1) makes, and obtains even gel in still aging 8 hours;
(5) after the even gel that step (4) is obtained removes free water, with deionized water solable matter in the filter cake is cleaned, again with gained solid vacuum freeze drying, maintain the temperature at-5 ℃ after the freeze-drying, be incubated 2 hours, grinding is sieved, and gets the ion sieve that graininess is removed aflatoxins.