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CN101366467A - Ion sieve for removing aflatoxin and preparation method thereof - Google Patents

Ion sieve for removing aflatoxin and preparation method thereof Download PDF

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Publication number
CN101366467A
CN101366467A CNA2008101522728A CN200810152272A CN101366467A CN 101366467 A CN101366467 A CN 101366467A CN A2008101522728 A CNA2008101522728 A CN A2008101522728A CN 200810152272 A CN200810152272 A CN 200810152272A CN 101366467 A CN101366467 A CN 101366467A
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China
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ratio
filtrate
ion sieve
deionized water
mass ratio
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CNA2008101522728A
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Chinese (zh)
Inventor
那平
刘洪佳
杨曙锋
曾方恒
郝玉荣
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Tianjin University
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Tianjin University
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Priority to CNA2008101522728A priority Critical patent/CN101366467A/en
Publication of CN101366467A publication Critical patent/CN101366467A/en
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Abstract

本发明公开了一种去除黄曲霉毒素的离子筛及制备方法,制备方法为:(1)将钠基蒙脱土加入去离子水中,浸泡成悬浮液;(2)将苯基三甲基溴化铵加入去离子水中,搅拌,过滤,得澄清滤液,备用;(3)将CuCl加入氨水中,搅拌,过滤得滤液,备用;(4)将步骤(2)及步骤(3)制得的滤液滴入步骤(1)制得的悬浮液中,静置陈化5-10小时得到均匀凝胶;(5)将均匀凝胶脱除游离水后,用去离子水将滤饼中可溶性物质洗净,再将所得固体真空冷冻干燥,冻干后保持温度在-10℃至0℃,保温1-3小时,研磨过筛,得颗粒状除黄曲霉素的离子筛。本发明的一种去除黄曲霉毒素的离子筛对黄曲霉素吸附速度快,吸附容量高。本发明制备方法简单。The invention discloses an ion sieve for removing aflatoxin and a preparation method thereof. The preparation method is as follows: (1) adding sodium-based montmorillonite into deionized water and soaking it into a suspension; (2) adding phenyl trimethyl bromide Add ammonium chloride into deionized water, stir, and filter to obtain a clarified filtrate for subsequent use; (3) add CuCl to ammonia water, stir, and filter to obtain a filtrate for subsequent use; (4) prepare the filtrate obtained in steps (2) and (3) The filtrate is dropped into the suspension prepared in step (1), and left to age for 5-10 hours to obtain a uniform gel; (5) after removing free water from the uniform gel, use deionized water to remove the soluble matter in the filter cake Washing, then vacuum freeze-drying the obtained solid, keeping the temperature at -10°C to 0°C after freeze-drying, keeping it warm for 1-3 hours, grinding and sieving to obtain a granular ion sieve for removing aflatoxin. The ion sieve for removing aflatoxin of the present invention has fast adsorption speed and high adsorption capacity for aflatoxin. The preparation method of the invention is simple.

Description

Remove the ion sieve and the preparation method of aflatoxin
Technical field
The present invention relates to a kind of ion sieve and preparation method, particularly relate to a kind of ion sieve and preparation method who removes aflatoxin.
Background technology
At present, remove that the most economical feasible method of aflatoxin is the physics detoxicity method in the food, commonly used has: extraction, absorption method, heat treating process and radiation method.Wherein, extraction is to use ethanol, and the acetone equal solvent comes out the aflatoxin extn in the food, only is applicable to the processing animal feed, and the expense height.Heat treating process is to make the aflatoxin molecular breakdown under HTHP, owing to need temperature very high, equipment is required height, expense height.Radiation method is to utilize infra-red radiation, and ultraviolet irradiation etc. destroy the molecular structure of aflatoxin, but strong ray also can destroy the structure of nutriment.At present used absorption method is to utilize adsorption of aflatoxin molecules such as aluminium silicate salt or zeolite, can reduce nutrient concentrations in the food but add this type of adsorbent in a large number.
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.

Claims (10)

1. ion sieve of removing aflatoxin is characterized in that making 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.
2. a kind of ion sieve of removing aflatoxin according to claim 1, it is characterized in that described 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.
3. a kind of ion sieve of removing aflatoxin according to claim 1 is characterized in that described step (2) is: the ratio in mass ratio 1:30 adds the phenyl trimethylammonium bromide in the deionized water, at 80r/min, stir 50min, filter, get clear filtrate, standby.
4. a kind of ion sieve of removing aflatoxin according to claim 1, it is characterized in that described 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, filter to get filtrate, standby.
5. a kind of ion sieve of removing aflatoxin according to claim 1, it is characterized in that described step (4) is: keeping mixing speed 80r/min, pH is 8, 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.
6. preparation method who removes the ion sieve of aflatoxin is characterized in that being 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.
7. a kind of preparation method who removes the ion sieve of aflatoxin according to claim 6, it is characterized in that described 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.
8. a kind of preparation method who removes the ion sieve of aflatoxin according to claim 6 is characterized in that described step (2) is: the ratio in mass ratio 1:30 adds the phenyl trimethylammonium bromide in the deionized water, at 80r/min, stir 50min, filter, get clear filtrate, standby.
9. a kind of preparation method who removes the ion sieve of aflatoxin according to claim 6, it is characterized in that described 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, filter to get filtrate, standby.
10. a kind of preparation method who removes the ion sieve of aflatoxin according to claim 6, it is characterized in that described step (4) is: keeping mixing speed 80r/min, pH is 8, 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.
CNA2008101522728A 2008-10-09 2008-10-09 Ion sieve for removing aflatoxin and preparation method thereof Pending CN101366467A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104692483A (en) * 2015-03-19 2015-06-10 王林双 Preparation method of compound ion sieve structure filter core
CN109364885A (en) * 2018-11-24 2019-02-22 烟台大学 Preparation method of sodium carboxymethyl cellulose-collagen-montmorillonite composite Aspergillus flavus adsorption material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104692483A (en) * 2015-03-19 2015-06-10 王林双 Preparation method of compound ion sieve structure filter core
CN109364885A (en) * 2018-11-24 2019-02-22 烟台大学 Preparation method of sodium carboxymethyl cellulose-collagen-montmorillonite composite Aspergillus flavus adsorption material
CN109364885B (en) * 2018-11-24 2021-03-12 烟台大学 Preparation method of sodium carboxymethylcellulose-collagen-montmorillonite composite aspergillus flavus adsorption material

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