CN103846078A - Preparation method of illite smectite mixed clay mycotoxin adsorbent - Google Patents
Preparation method of illite smectite mixed clay mycotoxin adsorbent Download PDFInfo
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Abstract
The invention discloses a preparation method of an illite smectite mixed clay mycotoxin adsorbent. The method comprises the steps of dissolving quaternary ammonium salt with carbon chains with different lengths into a water solution, and then adding illite smectite mixed clay for intercalation reaction; carrying out filter pressing on the product, and drying and grinding to obtain the illite smectite mixed clay mycotoxin adsorbent. The illite smectite mixed clay mycotoxin adsorbent is capable of effectively adsorbing multiple mycotoxins in feed, so that the feed conversion ratio is increased, the feed cost is reduced, and the health of livestock and poultry can be improved.
Description
Technical field
The present invention relates to feed additive field, be specifically related to a kind of preparation method of Yi Meng mixing clay mold toxin sorbent.
Background technology
Mycotoxin is a kind of ANFs being present in feed and raw material, is the mould secondary metabolite that toxin is very strong.It can cause: animal acute and chronic poisoning, reduce animal feed intake, and reduce production performance, feed conversion rate, the reproductive performance of animal, suppress animal immune function, meanwhile, mycotoxin also can be residual in animal products, for mankind's health care belt carrys out potential potential safety hazard.According to FAO (Food and Agriculture Organization of the United Nation) statistics, the whole world approximately has 25% cereal to be subject to the pollution of mycotoxin in various degree, has the grain of 5%-7% and feed to lose feeding value because go mouldy.In modern times cultivation, every year because processing mycotoxin to the economic loss of bringing more than one hundred million units in Production of Livestock and Poultry.Therefore, finding that suitable effective method controls it is the task of top priority of animal husbandry development.
To detoxicating mycotoxin, processing mainly contains at present: the methods such as mechanical detoxification, biological detoxication, chemical detoxication and physical absorption detoxification.Absorption detoxicity method is both economical, effective and has the method for realistic meaning, it is the polar functional group that attracts mycotoxin by adsorbent, by their absorption, catch and fix, stop the absorption of body contratoxin, thus residual in agricultural product of the harm of reduction toxin to body and toxin.Absorption detoxicity method is promoted in a big way in production practices, and in prior art, conventional adsorbent has hydration ca aluminosilicate sodium salt (HSCAS), montmorillonite, zeolite and active carbon etc.But the relevant report of applying in feed additive field so far there are no Yi Meng mixing clay.
Yi Meng mixing clay is neither illite, neither montmorillonite, but by illite (hydromica 30～70%) and two kinds of clay mineral compositions of montmorillonite (bentonite 20～49%), there is the special performance of two kinds of mineral.Owing to having illite and montmorillonite simultaneously, there is unique natural micro nano structure and stronger adsorptivity and good suspension, dispersiveness, obtained application at aspects such as bactericidal suspending agent (CN 102742573 A), decolorizer (CN 103007876 A) and adhesives (CN 103484027 A).
The Yi Meng mixing clay of natural output has hydrophilic negative surface charge, and to having the mycotoxin of polar group, as aflatoxin has stronger absorption property, but the mycotoxin weak to polarity (as zearalenone etc.) adsorption capacity is limited.
Summary of the invention
The object of the invention is: the preparation method that a kind of Yi Meng mixing clay mold toxin sorbent is provided, adopt the quaternary ammonium salt of different length carbochain to carry out organically-modified to Yi Meng mixing clay, prepare Yi Meng mixing clay mold toxin sorbent by the degree organising that changes surfactant, overcome the deficiency of natural Yi Meng mixing clay in feed applications, improve the adsorption effect of Yi Meng clay, strengthen the adsorption capacity to low pole mycotoxin, further expand the absorbed species of contratoxin.
Technical solution of the present invention is that the preparation method of this Yi Meng mixing clay mold toxin sorbent is as follows: first the quaternary ammonium salt of different length carbochain is dissolved in the aqueous solution, then add Yi Meng mixing clay at 60 ~ 100 DEG C of reaction 4 ~ 12 h, naturally be cooled to room temperature, press filtration, dry, pulverize, obtain Yi Meng mixing clay mold toxin sorbent.
Wherein, the quaternary ammonium salt of described different length carbochain is any in DTAB, TTAB, softex kw, Cetyltrimethylammonium bromide, two Cetyltrimethylammonium bromide, and consumption is 0.1 ~ 5 times of Yi Meng mixing clay cation exchange capacity.
Wherein, described Yi Meng mixing clay is natural formation, and its cation exchange capacity is greater than 20mmol/100g, pulverizes 200 orders before use.
The present invention has the following advantages:
(1) the quaternary ammonium salt-modified Yi Meng mixing clay of employing different length carbochain, by control surface activating agent kind, consumption, reaction temperature, formation has the Yi Meng mixing clay that organises of different surfaces hydrophobicity, in efficient adsorption polarity mycotoxin, improve the adsorption effect to low pole mycotoxin, thereby obtain Yi Meng mixing clay mold toxin sorbent efficient, wide spectrum.
(2) by the intercalation of cation organic surface active agent to Yi Meng mixing clay, not only expanded the interlamellar spacing of Yi Meng mixing clay, and changed the surface charge of Yi Meng mixing clay, thereby improved the adsorbance of low pole mycotoxin.
(3) the organically-modified mild condition of Yi Meng mixing clay, technical process is simple, is easy to accomplish scale production.
Brief description of the drawings
Fig. 1 is (0.25E, 1E and 1.5E) infrared spectrogram of Yi Meng mixing clay and softex kw modification Yi Meng mixing clay mold toxin sorbent.
Detailed description of the invention
In order better technical scheme of the present invention being described, further to describe by the following examples, and be not limited to embodiment.
embodiment 1:the DTAB that takes 5 times of cation exchange capacities of Yi Meng mixing clay, is dissolved in suitable quantity of water, then adds Yi Meng mixing clay to be mixed with the slurries of 5% mass concentration, then, at 60 DEG C of reaction 12h, product is filtered, and washing, uses AgNO
3inspection is without after Br-, and press filtration, dry, pulverizing, obtain modification Yi Meng mixing clay mold toxin sorbent.This adsorbent is respectively 100 and 82% to the external clearance of aspergillus flavus toxin and zearalenone.
embodiment 2:the TTAB that takes 2 times of cation exchange capacities of Yi Meng mixing clay, is dissolved in suitable quantity of water, then adds Yi Meng mixing clay to be mixed with the slurries of 5% mass concentration, then, at 75 DEG C of reaction 6h, product is filtered, and washing, uses AgNO
3inspection is without after Br-, and press filtration, dry, pulverizing, obtain modification Yi Meng mixing clay mold toxin sorbent.This adsorbent is respectively 100 and 78% to the external clearance of aspergillus flavus toxin and zearalenone.
embodiment 3:the softex kw that takes 1.5 times of cation exchange capacities of Yi Meng mixing clay, is dissolved in suitable quantity of water, then adds Yi Meng mixing clay to be mixed with the slurries of 5% mass concentration, then, at 80 DEG C of reaction 4h, product is filtered, and washing, uses AgNO
3inspection is without after Br-, and press filtration, dry, pulverizing, obtain modification Yi Meng mixing clay mold toxin sorbent.This adsorbent is respectively 100 and 85% to the external clearance of aspergillus flavus toxin and zearalenone.
embodiment 4:the Cetyltrimethylammonium bromide that takes 1 times of cation exchange capacity of Yi Meng mixing clay, is dissolved in suitable quantity of water, then adds Yi Meng mixing clay to be mixed with the slurries of 5% mass concentration, then, at 80 DEG C of reaction 8h, product is filtered, and washing, uses AgNO
3inspection is without after Br-, and press filtration, dry, pulverizing, obtain modification Yi Meng mixing clay mold toxin sorbent.This adsorbent is respectively 100 and 72% to the external clearance of aspergillus flavus toxin and zearalenone.
embodiment 5:the two Cetyltrimethylammonium bromides that take 0.1 times of cation exchange capacity of Yi Meng mixing clay, are dissolved in suitable quantity of water, then add Yi Meng mixing clay to be mixed with the slurries of 5% concentration, then, at 100 DEG C of reaction 6h, product are filtered, and washing, uses AgNO
3inspection is without after Br-, and press filtration, dry, pulverizing, obtain modification Yi Meng mixing clay mold toxin sorbent.This adsorbent is respectively 100 and 68% to the external clearance of aspergillus flavus toxin and zearalenone.
As shown in Figure 1, be the infrared spectrogram of the Yi Meng mixing clay mold toxin sorbent of Yi Meng mixing clay and softex kw modification, as seen from the figure, at 2924,2851 and 1473 cm
-1there is new absworption peak, the other Biao Shi of this Fen – CH in place
3he – CH
2asymmetric stretching vibration, symmetrical stretching vibration and flexural vibrations, in addition, the intensity at peak strengthens along with the increase of degree of organising, and illustrates that Yi Meng mixing clay is by organically-modified.
Claims (4)
1. the preparation method of Yi Meng mixing clay mold toxin sorbent, it is characterized in that: first the quaternary ammonium salt of different length carbochain is dissolved in the aqueous solution, then add Yi Meng mixing clay at 60 ~ 100 DEG C of reaction 4 ~ 12 h, naturally be cooled to room temperature, press filtration, dry, pulverize, obtain Yi Meng mixing clay mold toxin sorbent.
2. the preparation method of Yi Meng mixing clay mold toxin sorbent according to claim 1, is characterized in that: the quaternary ammonium salt of different length carbochain is any in DTAB, TTAB, softex kw, Cetyltrimethylammonium bromide, two Cetyltrimethylammonium bromide.
3. the preparation method of Yi Meng mixing clay mold toxin sorbent according to claim 1, is characterized in that: the consumption of the quaternary ammonium salt of different length carbochain is 0.1 ~ 5 times of Yi Meng mixing clay cation exchange capacity.
4. the preparation method of Yi Meng mixing clay mold toxin sorbent according to claim 1, is characterized in that: Yi Meng mixing clay is natural formation, and cation exchange capacity is greater than 20mmol/100g, pulverizes 200 orders before use.
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Cited By (10)
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| CN104888691A (en) * | 2015-05-29 | 2015-09-09 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of antibacterial attapulgite zearalenone adsorbent |
| CN106179194A (en) * | 2016-07-06 | 2016-12-07 | 浙江丰虹新材料股份有限公司 | A kind of modified clay and its preparation method and application |
| CN106732465A (en) * | 2017-02-22 | 2017-05-31 | 李峰 | A kind of composite type water treating agent of efficient absorption methyl orange dye |
| CN106824109A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of modified chitin gel ball cooperates with the enhanced heavy metal absorbent of lemon dregs adsorption effect |
| CN106824130A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
| CN107159140A (en) * | 2017-06-05 | 2017-09-15 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The preparation method of organo-mineral complexing attapulgite mold toxin sorbent |
| CN109647339A (en) * | 2019-01-25 | 2019-04-19 | 中国科学院兰州化学物理研究所 | The method for preparing mold toxin sorbent using semicoke |
| CN109647347A (en) * | 2019-01-23 | 2019-04-19 | 东北农业大学 | Albite zearalenone adsorbent and preparation method thereof |
| CN114259982A (en) * | 2021-12-31 | 2022-04-01 | 南宁师范大学 | Zinc oxide silicon-based pillared illite-montmorillonite clay composite material and preparation method and application thereof |
| CN115428885A (en) * | 2021-06-02 | 2022-12-06 | 菲吉乐科(南京)生物科技有限公司 | Broad-spectrum mildew removing agent capable of simultaneously adsorbing mycotoxin, endotoxin and enterotoxin |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104888691A (en) * | 2015-05-29 | 2015-09-09 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of antibacterial attapulgite zearalenone adsorbent |
| CN106179194A (en) * | 2016-07-06 | 2016-12-07 | 浙江丰虹新材料股份有限公司 | A kind of modified clay and its preparation method and application |
| CN106732465A (en) * | 2017-02-22 | 2017-05-31 | 李峰 | A kind of composite type water treating agent of efficient absorption methyl orange dye |
| CN106824109A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of modified chitin gel ball cooperates with the enhanced heavy metal absorbent of lemon dregs adsorption effect |
| CN106824130A (en) * | 2017-02-22 | 2017-06-13 | 李峰 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
| CN107159140A (en) * | 2017-06-05 | 2017-09-15 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The preparation method of organo-mineral complexing attapulgite mold toxin sorbent |
| CN109647347A (en) * | 2019-01-23 | 2019-04-19 | 东北农业大学 | Albite zearalenone adsorbent and preparation method thereof |
| CN109647339A (en) * | 2019-01-25 | 2019-04-19 | 中国科学院兰州化学物理研究所 | The method for preparing mold toxin sorbent using semicoke |
| CN115428885A (en) * | 2021-06-02 | 2022-12-06 | 菲吉乐科(南京)生物科技有限公司 | Broad-spectrum mildew removing agent capable of simultaneously adsorbing mycotoxin, endotoxin and enterotoxin |
| CN114259982A (en) * | 2021-12-31 | 2022-04-01 | 南宁师范大学 | Zinc oxide silicon-based pillared illite-montmorillonite clay composite material and preparation method and application thereof |
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Effective date of registration: 20210812 Address after: 730013 No.18 Tianshui Middle Road, Chengguan District, Lanzhou City, Gansu Province Patentee after: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences Address before: 211700 No. 3 Dongfang Avenue, Xucheng Town, Xuyi county, Huai'an City, Jiangsu Province Patentee before: XUYI R & D CENTER FOR APPLICATION OF ATTAPULGITE CLAY, LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES |