CN1123380C - Self-controlled oxygen absorbent and its prepn - Google Patents
Self-controlled oxygen absorbent and its prepn Download PDFInfo
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- CN1123380C CN1123380C CN 01114850 CN01114850A CN1123380C CN 1123380 C CN1123380 C CN 1123380C CN 01114850 CN01114850 CN 01114850 CN 01114850 A CN01114850 A CN 01114850A CN 1123380 C CN1123380 C CN 1123380C
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Abstract
The present invention discloses a self control type oxygen absorbent and a preparation method thereof. The oxygen absorbent is prepared from iron powder, strong water absorbents, active carbon, nontoxic alkali metal or alkaline earth metal halogenide and water according to a definite proportion. The oxygen absorbent can effectively inhibit the growth of microorganisms, such as bacteria, mycete, etc. under a closed condition, can prevent mildewing, infesting, oxidizing and degenerating, and can be used for sealing and storing grains, processed food, dried fruit, dried vegetables, marine products, condiments, sauted goods, tea leaves, tobacco leaves, optical instruments, electronic elements, medicinal materials, textiles, fur goods, precise machines, roll films, books, pictures, cultural relics, files, etc.
Description
Affiliated technical field
The present invention relates to a kind of self-controlled oxygen absorbent that is used to seal up for safekeeping article such as varieties of food items, grain, medicine, archives, electronic device, optical component, the invention still further relates to the preparation method of this self-controlled oxygen absorbent.
Background technology
Oxygen absorbent is deoxidier or oxygen scavenger again, easily and the free oxygen generation steady oxide that reacts.Oxygen absorbent is sealed in the packing container with sealing up for safekeeping article, can absorbs the oxygen in the container, thereby prevent to be sealed the oxidation of article, suppress the breeding of aerobic microorganism and worm, thereby reach the preservation purpose of being sealed up for safekeeping article.With regard to the raw materials used difference of oxygen absorbent, divide mineral-type and organic class two big classes.Mineral-type is generally iron powder or sodium dithionite, and organic class is generally ascorbic acid or catechol.The redox reaction of iron and oxygen is a micro cell reaction system, could carry out smoothly there being power and water to separate under the situation that matter exists redox reaction, and temperature can be accelerated its reaction speed.General is the oxygen absorbent of raw material with the iron powder, and prescription is mainly mixed by A and B two big components.Component A is an Oxygen body, is that the iron powder and the metal halide aqueous solution fully mix, and makes metal halide coat the iron powder surface, and drying forms again; B component is an oxygen uptake control composition, also can be described as the carrier water supplying system, is mainly suitable carrier and the metal halide aqueous solution evenly mixes.The carrier that adopts is the porous micro mist at present, as zeolite, kaolin, loess, diatomite, bentonite, carclazyte, active carbon, silica, aluminium oxide, silica gel etc., " Ageless " oxygen absorbent of producing as the famous gas company of Mitsubishi of Japan, with zeolite as filler.People's (seeing CN85100834U) such as the Zhang Yaxing of China the No. 8511 Research Institute of the Minsistry of space Industry propose also available rice hull ash as carrier.But above-mentioned oxygen absorbent also exposes some problems in producing the practice of using, as:
(1) oxygen absorption rate of common oxygen absorbent generally is gesture first quick and back slow, be that oxygen uptake is reacted when just having begun, because the abundance of Fe powder and water, the oxygen uptake reaction is carried out very soon, and along with the intensification of the extent of reaction, the amount of Fe powder reduces thereupon, because the rising moisture of system temperature also has part to scatter and disappear, the oxygen uptake reaction speed can be slack-off, even can cause the waste of iron powder owing to moisture loss excessively can not make the iron powder complete reaction, this oxygen uptake reaction characteristics have first quick and back slow brought very burden for the preparing process of oxygen absorbent and concrete the use, to the time requirement strictness that is mixed, have influenced manufacturability, and in necessary the subcontracting in the time of concrete use, oxygen absorbent is heating rapidly just, has brought great inconvenience to the user, and " reserve strength " deficiency also seems again when really needing " oxygen uptake " reaction beginning.
(2) common oxygen absorbent oxygen uptake reaction pair environment temperature descends influences sensitivity, and when environment temperature was lower than 15 ℃, oxygen absorption rate obviously reduced, when temperature is reduced to 10 ℃ of left and right sides, reaction almost stops, and like this, just can not normally bring into play the effect that oxygen uptake is sealed up for safekeeping in winter under the environment.
Summary of the invention
The object of the present invention is to provide the self-controlled oxygen absorbent that a kind of oxygen absorption rate is " starting autoacceleration slowly ", temperature influence is little, oxygen uptake is effective.
Another object of the present invention also is to provide the preparation method of this self-controlled oxygen absorbent.
Self-controlled oxygen absorbent provided by the invention, its component and content (weight) are:
The iron powder 25～80% that 20 orders are above
Super strength water absorbent 0.5～10%
Activated carbon 5～50%
Nontoxic alkali metal or alkaline-earth halide 1～8%
Water 3～28%.
The preferred ingredient and the content (weight) of preparation chemical oxygen absorbent of the present invention are:
The iron powder 40～70% that 50 orders are above
Super strength water absorbent 1～5%
Activated carbon 10～25%
Nontoxic alkali metal or alkaline-earth halide 2.5～5%
Water 5～25%.
The optimal component and the content (weight) of preparation chemical oxygen absorbent of the present invention are:
The iron powder 45～60% that 80 orders are above
Super strength water absorbent 1～3%
Activated carbon 15～25%
Nontoxic alkali metal or alkaline-earth halide 3～4%
Water 8～25%.
The method that above-mentioned each component is made chemical oxygen absorbent of the present invention is:
(1) iron powder, super strength water absorbent and activated carbon are mixed in proportion;
(2) nontoxic alkali metal or alkaline-earth halide is water-soluble, make the aqueous solution;
(3) aqueous solution that step (2) is made adds in the mixture of step (1), stirs, and promptly makes this chemical oxygen absorbent.
Self-controlled oxygen absorbent of the present invention is formulated by a certain percentage by iron powder, super strength water absorbent, activated carbon, nontoxic alkali metal or alkaline-earth halide and water, is feature with the black particle mixed structure, and product is a bronzing.
Iron powder is the most basic, a topmost component in the self-controlled oxygen absorbent prescription, and what of iron content the height of its ability to take oxygen fundamentally be decided by.Self-controlled oxygen absorbent is not strict with the source of iron powder, and reduced iron powder, electrolytic iron powder, atomized iron powder, the cast iron powder that contains certain impurity all can be used as component raw material.The order number of iron powder should be preferably in more than 80 orders more than 20 orders.
Super strength water absorbent is one of another important component of self-controlled oxygen absorbent, and the completeness of its oxygen absorption rate, oxygen uptake reaction all has direct relation with the content of super strength water absorbent.Super strength water absorbent among the present invention is meant the material that a kind of water absorbing capacity is strong especially, and its water absorption is self tens times and extremely several thousand times, and not only water absorbing capacity is extremely strong for it, and water holding capacity is also very high, and therefore, it also can be high water-loss reducer.Super strength water absorbent in the self-controlled oxygen absorbent is high molecular polymer low crosslinking degree or partially crystalline that has many hydrophilic radicals, is that water-soluble high-molecular compound carries out crosslinked and gets, and mainly has following characteristics from a structural point:
(1) thing is a cross-linked type macromolecule, and is generally insoluble in solvent, swelling rapidly after the suction, and volume increases manyfold, because water is wrapped in and is gelatinous molecular network inside, is difficult for running off and volatilization.
(2) have the strongly hydrophilic group in the molecule, as hydroxyl, carboxyl etc., polymer molecule can form hydrogen bond or other chemical bond with hydrone, therefore strong polar substances such as water is had the certain surface adsorption capacity.
(3) super strength water absorbent generally has special stereochemical structure, and the back that helps absorbing water keeps certain mechanical strength, keeps moisture.
Super strength water absorbent is meant the high molecular polymer with above-mentioned feature among the present invention, mainly comprises following three big series:
1, starch series is as starch-grafted acrylonitrile type, starch grafted acrylate type, starch graft acrylamide type, starch carboxymethylation reaction type, starch xanthate grafted propylene hydrochlorate type, starch acrylamide acid graft copolymerization, the acid amide-grafted copoly type of starch acrylamide, starch maleic three acid anhydride-grafted copoly types etc.
2, cellulose series is intersected cross-linking type etc. as epoxychloropropane after carboxymethyl cellulose type, cellulose (or CMC) grafted propylene nitrile type, cellulose (or CMC) grafted propylene acid type, cellulose xanthogenation grafted propylene hydrochlorate type, cellulose (or CMC) graft acrylamide type, the carboxymethyl celluloseization.
3, synthetic resin series is as polyacrylate type, polyacrylamide type, acrylate and vinyl acetate copolymerized type, acrylic acid and acrylamide copoly type, polyvinyl alcohol-acid anhydrides copolymerzation with cross-linking type, polyvinyl alcohol-acrylic graft copolymer type, vinyl acetate-acrylic ester copolymer hydrolysis-type, vinyl acetate-maleic anhydride copoly type, polyoxy support system etc.
At the above-mentioned all kinds of super strength water absorbents that can be used for self-controlled oxygen absorbent, be the best with the super strength water absorbent of salt tolerant type.
Activated carbon also is one of solvent in the self-controlled oxygen absorbent.Activated carbon is the material of a class porous tool adsorption property, and it can increase the surface area of whole system, increases gas permeability, makes oxygen form higher density around iron, thereby can improve ability to take oxygen and oxygen absorption rate.Activated carbon also has the effect of dispersant simultaneously.
Metal halide in the self-controlled oxygen absorbent plays the effect of transmitting electronics in the micro cell of oxygen uptake reaction, its content is very big to the influence of oxygen absorption rate and ability to take oxygen.Nontoxic alkali metal or the alkaline-earth halide of the general employing of metal halide in the self-controlled oxygen absorbent is wherein with the very good sodium chloride the best of security.
Moisture is the necessary condition of oxygen uptake reaction, does not have reaction of moisture to carry out with regard to difficulty, and can whether moisture have also determined the speed of oxygen uptake reaction speed and oxygen uptake reaction react thorough in right amount.Self-controlled oxygen absorbent reaches the automatic control purpose of oxygen absorption rate just to the control of moisture rate of release by super strength water absorbent.As the above, super strength water absorbent all has natural or synthetic polymer three-dimensional cross-linked structure, the suction-operated of strong hydrophilicity group and water is strong in the water absorbing agent, be easy to swelling by water institute, and the three-dimensional structure of crosslinked formation stops the dissolving of super strength water absorbent, therefore constitutes the spawn that contains big water gaging.Begin oxygen uptake when reaction when oxygen absorbent runs into oxygen, required moisture from the network structure of super strength water absorbent at leisure desorption come out because the rate of release of moisture is very slow, so the oxygen uptake of self-controlled oxygen absorbent reaction has the characteristics of " starting slowly ".Along with the carrying out of oxygen uptake reaction, iron powder changes ferric ion into by iron atom, and the generation of iron ion plays catalytic action to super strength water absorbent to the rate of release of moisture, thereby has caused the gesture of " autoacceleration " of oxygen uptake reaction.
Self-controlled oxygen absorbent of the present invention can be used for sealing up for safekeeping article such as grain, processed food, dry fruit, dried vegetable, marine products category, seasoning class, roasted seeds and nuts, tealeaves, tobacco leaf and optical instrument, electronic component, medicinal material, textile, fur goods, precision optical machinery, film, painting and calligraphy, historical relic, archives, be the renewal product of common oxygen absorbent, its advantage is as follows:
(1) the oxygen uptake reaction speed of self-controlled oxygen absorbent is the gesture of " starting slowly; autoacceleration ", promptly in the beginning several hrs, the oxygen uptake sluggish is carried out, promptly " start slowly ", intensification along with the oxygen uptake extent of reaction, reaction is the gesture of " autoacceleration ", it is the middle and later periods that the best point of oxygen absorption rate appears at the oxygen uptake process, this has just brought convenience for the preparation of oxygen absorbent and use, the time of subcontracting has been reserved bigger space in give using, and has overcome common oxygen absorbent and have " reserve strength " not enough shortcoming.
(2) self-controlled oxygen absorbent is subjected to Temperature Influence little, even below 10 ℃, oxygen absorption rate also just slows down slightly, and not like common oxygen absorbent, the reaction of oxygen uptake below 10 ℃ almost can not normally be carried out and deoxidation fully.
(3) water-retaining property of self-controlled oxygen absorbent is strong, and shelf characteric is stable, can not lose moisture in depositing process, also unnecessary steam in the packing can be sucked back the oxygen absorbent system, so just can not influence the carrying out that holds the oxygen uptake reaction of bag back owing to the forfeiture of moisture.
(4) self-controlled oxygen absorbent reduces the requirement of iron powder, does not need to do specially treated, and iron powder needs to do special activation processing under vacuum condition in common oxygen absorbent.
(5) the ability to take oxygen height of self-controlled oxygen absorbent, its oxygen absorbed are 2～3 times of common oxygen absorbent same model product.
(6) self-controlled oxygen absorbent is non-pulverous black particle component, can not spill and contaminated food products from the micropore of packaging bag in storing and using.
Describe the present invention in detail below by embodiment.
Embodiment 1
100g reduced iron powder, 5g Sodium Polyacrylate type super strength water absorbent and 20g activated carbon are mixed; under nitrogen protection, slowly add 20% sodium chloride solution 30ml while stirring; after stirring; under nitrogen atmosphere, use the packing of gas permeability composite material film; every 3g is one bag, makes pouch dress oxygen absorbent.
The above-mentioned pouch of taking is adorned one bag of oxygen absorbent, measures its total oxygen absorbed with the special device of measuring oxygen absorbed, and after 72 hours, total oxygen absorbed is more than 300ml.
Take one bag of above-mentioned oxygen absorbent places 1.5 liters closed container, and the oxygen concentration that records in the container with oxygen analyser after 24 hours is reduced to below 0.1%.
Embodiment 2
Prepared oxygen absorbent among the embodiment 1 is placed in the brand new 175g guang-type moon cake packaging bag (packaging bag for resistance oxygen KOP/PE complex pocket) preferably seal together with moon cake, blank sample is promptly seen mildew after 15 days, the moon cake that is placed with oxygen absorbent did not still have mouldy in three months.
Embodiment 3
50kg iron powder, 2.5kg starch grafted acrylate type super strength water absorbent and the 12kg activated carbon back that stirs is added 20% sodium chloride solution 15kg while stirring under nitrogen protection; after adding sodium chloride solution; stir half an hour again; assurance stirs; pocket coating-dividing sealing with brown paper is made promptly makes this self-controlled oxygen absorbent.
Embodiment 4
In common room formula silo, spread tensile nylon/polyethylene film and make bottom, on bottom 150 tons of packing rice compact reactors being become volume is the big buttress of 188 cubic metres (long * wide * high=11.2 meters * 4.8 meters * 3.5 meters), lay the oxygen absorbent that makes by embodiment 3 then around buttress, to count 4 general oxygen indicator and place easy observed place, immediately the big tent of ready tensile nylon/polyethylene is put, with heat seal tool bottom and big tent are tightly sealed, confirm the ne-leakage part, oxygen indicator reddens in one week, seals up for safekeeping promptly and finishes.
Embodiment 5
24kg iron powder, 1.2kg cellulose graft acrylonitrile type super strength water absorbent and the 5.5kg activated carbon back that stirs is added 20% sodium chloride solution 7kg while stirring under nitrogen protection; after adding sodium chloride solution; stir half an hour again; assurance stirs; under nitrogen atmosphere, use the packing of gas permeability composite material film; every 6g is one bag, makes pouch dress oxygen absorbent.
The above-mentioned pouch of taking is adorned one bag of oxygen absorbent, measures its total oxygen absorbed with the special device of measuring oxygen absorbed, and after 72 hours, total oxygen absorbed is more than 600ml.
Take one bag of above-mentioned oxygen absorbent places 3 liters closed container, and the oxygen concentration that records in the container with oxygen analyser after 24 hours is reduced to below 0.1%.Embodiment 6
30kg iron powder, 1.5kg polyacrylamide type super strength water absorbent and the 8kg activated carbon back that stirs is added 20% sodium chloride solution 9kg while stirring under nitrogen protection; after adding sodium chloride solution; stir half an hour again; assurance stirs; under nitrogen atmosphere, use the packing of gas permeability composite material film; every 2g is one bag, makes pouch dress oxygen absorbent.
The above-mentioned pouch of taking is adorned one bag of oxygen absorbent, measures its total oxygen absorbed with the special device of measuring oxygen absorbed, and after 72 hours, total oxygen absorbed is more than 180ml.
Take one bag of above-mentioned oxygen absorbent places 0.5 liter closed container, and the oxygen concentration that records in the container with oxygen analyser after 24 hours is reduced to below 0.1%.
Embodiment 7
50kg iron powder, 2.5kg acrylic acid and acrylamide copoly type super strength water absorbent and the 12kg activated carbon back that stirs is added 20% sodium chloride solution 14kg while stirring under nitrogen protection; after adding sodium chloride solution; stir half an hour again; assurance stirs; under nitrogen atmosphere, use the packing of gas permeability composite material film; every 1kg is one bag, makes packed oxygen absorbent.
With one bag of above-mentioned packed oxygen absorbent and a slice oxygen indicator, with a load tobacco sealed after being vacuumized (outer packaging bag for resistance oxygen K nylon/PE complex pocket) preferably, oxygen indicator reddens after three days, and the sealing up for safekeeping promptly to accuse of tobacco finished.
Claims (10)
1, a kind of self-controlled oxygen absorbent, its component and content (weight) are:
The iron powder 25～80% that 20 orders are above
Super strength water absorbent 0.5～10%
Activated carbon 5～50%
Nontoxic alkali metal or alkaline-earth halide 1～8%
Water 3～28%.
2, self-controlled oxygen absorbent according to claim 1, its component and content (weight) are
The iron powder 40～70% that 50 orders are above
Super strength water absorbent 1～5%
Activated carbon 10～25%
Nontoxic alkali metal or alkaline-earth halide 2.5～5%
Water 5～25%.
3, self-controlled oxygen absorbent according to claim 1, its component and content (weight) are
The iron powder 45～60% that 80 orders are above
Super strength water absorbent 1～3%
Activated carbon 15～25%
Nontoxic alkali metal or alkaline-earth halide 3～4%
Water 8～25%.
4, self-controlled oxygen absorbent according to claim 1 is characterized in that: described iron powder is meant reduced iron powder, electrolytic iron powder, atomized iron powder that general industry is used or the cast iron powder that certain impurity is arranged.
5, according to the self-controlled oxygen absorbent of claim described 1, it is characterized in that: described super strength water absorbent is meant high molecular polymer low crosslinking degree or partially crystalline that has many hydrophilic radicals, and can absorb the macromolecular material that is higher than the own wt several times rapidly after water contacts.
6, according to the self-controlled oxygen absorbent of claim described 5, it is characterized in that: described super strength water absorbent is a starch series, comprises starch-grafted acrylonitrile type, starch grafted acrylate type, starch graft acrylamide type, starch carboxymethylation reaction type, starch xanthate grafted propylene hydrochlorate type, starch acrylamide acid graft copolymerization, the acid amide-grafted copoly type of starch acrylamide or starch maleic three acid anhydride-grafted copoly types.
7, according to the self-controlled oxygen absorbent of claim described 5, it is characterized in that: described super strength water absorbent is a cellulose series, comprises after carboxymethyl cellulose type, cellulose graft acrylonitrile type, cellulose graft acrylic type, cellulose xanthogenation grafted propylene hydrochlorate type, cellulose graft acid/acrylic amide type or the carboxymethyl celluloseization that epoxychloropropane intersects cross-linking type.
8, according to the self-controlled oxygen absorbent of claim described 5, it is characterized in that: described super strength water absorbent is a synthetic resin series, comprises polyacrylate type, polyacrylamide type, acrylate and vinyl acetate copolymerized type, acrylic acid and acrylamide copoly type, polyvinyl alcohol-acid anhydrides copolymerzation with cross-linking type, polyvinyl alcohol-acrylic graft copolymer type, vinyl acetate-acrylic ester copolymer hydrolysis-type, vinyl acetate-maleic anhydride copoly type or polyoxy support system.
9, self-controlled oxygen absorbent according to claim 1 is characterized in that: described nontoxic alkali metal or alkaline-earth halide are commercially available refining sodium chloride.
10, the preparation method of the described self-controlled oxygen absorbent of claim 1, this method may further comprise the steps:
(1) iron powder, super strength water absorbent and activated carbon are mixed in proportion;
(2) nontoxic alkali metal or alkaline-earth halide is water-soluble, make the aqueous solution;
(3) aqueous solution that step (2) is made adds in the mixture of step (1), stirs, and promptly makes this chemical oxygen absorbent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01114850 CN1123380C (en) | 2001-06-26 | 2001-06-26 | Self-controlled oxygen absorbent and its prepn |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01114850 CN1123380C (en) | 2001-06-26 | 2001-06-26 | Self-controlled oxygen absorbent and its prepn |
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| CN1337273A CN1337273A (en) | 2002-02-27 |
| CN1123380C true CN1123380C (en) | 2003-10-08 |
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| CN 01114850 Expired - Fee Related CN1123380C (en) | 2001-06-26 | 2001-06-26 | Self-controlled oxygen absorbent and its prepn |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100403908C (en) * | 2006-09-16 | 2008-07-23 | 华通(常州)生化有限公司 | Pollution-free tobacco mellowing and mildew-proof pesticide |
| CN101904541B (en) * | 2010-08-04 | 2012-10-17 | 广东广益科技实业有限公司 | Deoxidizing preservative and preparation method thereof |
| CN102319556A (en) * | 2011-06-15 | 2012-01-18 | 金川集团有限公司 | Oxygen absorbent for preventing oxidization of metal powder |
| CN103007880B (en) * | 2012-11-30 | 2014-11-05 | 深圳市海格金谷化工科技有限公司 | Carbon deoxidizer and preparation method thereof |
| CN104415658A (en) * | 2013-09-10 | 2015-03-18 | 湖南华望熏蒸消毒有限公司 | Chemical gas regulating agent and preparation method thereof |
| CN103478247B (en) * | 2013-09-11 | 2015-02-25 | 杭州巨炬科技有限公司 | Iron-series deoxidizing agent |
| CN105053752A (en) * | 2015-07-22 | 2015-11-18 | 小嵩保鲜技术(常熟)有限公司 | Deoxidizer and production technology thereof |
| CN106669632A (en) * | 2017-01-16 | 2017-05-17 | 苏州苏米欧贸易有限公司 | Environment-friendly desiccant |
| CN107837646B (en) * | 2017-11-28 | 2023-07-28 | 江苏科威环保技术有限公司 | Multi-component organic waste gas safety treatment device and process thereof |
| CN108338308B (en) * | 2018-01-03 | 2022-06-07 | 广东广益科技实业有限公司 | Preservative with double-suction function and preparation method thereof |
| CN108464430A (en) * | 2018-04-09 | 2018-08-31 | 袁国森 | A kind of food desiccant and preparation method thereof |
| JP7363099B2 (en) * | 2019-05-24 | 2023-10-18 | 三菱瓦斯化学株式会社 | Oxygen scavenger composition and method for producing the same |
| CN112821010A (en) * | 2021-01-30 | 2021-05-18 | 九江冠力新材料有限公司 | Low-moisture ceramic diaphragm, preparation method and lithium battery |
| CN114009492A (en) * | 2021-11-17 | 2022-02-08 | 东莞市欣荣天丽科技实业有限公司 | Cooked gel-like preservative and preparation method thereof |
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