CN101045790A - Synthesis method of shell starch microsphere - Google Patents

Synthesis method of shell starch microsphere Download PDF

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Publication number
CN101045790A
CN101045790A CNA2007100177641A CN200710017764A CN101045790A CN 101045790 A CN101045790 A CN 101045790A CN A2007100177641 A CNA2007100177641 A CN A2007100177641A CN 200710017764 A CN200710017764 A CN 200710017764A CN 101045790 A CN101045790 A CN 101045790A
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parts
mixture
starch
gel
tween60
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CN100462391C (en
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王磊
李仲谨
韩敏
陈丽
田颖
王景平
黄凤芹
赵强
刘节根
刘宝华
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Shaanxi University of Science and Technology
Shaanxi University of Technology
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Shaanxi University of Science and Technology
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  • Manufacturing Of Micro-Capsules (AREA)
  • Cosmetics (AREA)

Abstract

This invention relates to a synthetic method of hud type starch microsphere. First carry out fully microwave dispersing to titanium dioxide, sodium silicate and de-ionized water, obtain TiO2 gel; blend soluble starch and de-ionized water, gain starch solution; intensive mixing cyclohexane, initiator, emulsifying agent, add TiO2 gel, then add cross-linking agent N, N -methylene bisacrylamide and starch solution, take reaction for 3 to 4 hours; finally stop whip, cooling, standing, by centrifugal to remove oil phase; use ethyl acetate, acetone, dehydrated alcohol in turns and abundantly to wash obtained precipitate, gain white go as far as yellowish product, vacuum drying.

Description

The synthetic method of shell starch microsphere
Technical field
The present invention relates to a kind of synthetic method of spherex, be specifically related to a kind of synthetic method of shell starch microsphere.
Background technology
Present complex microsphere, generated time long (generally needing more than 10 hours), monomer that it is used and auxiliary agent price are also higher, thereby cost is too high, and it can only be used as the carrier of medicine for a long time, and can't fully be used in other field.Traditional sol-gel technology is a raw material with expensive titanium alkoxide normally, adds the hydrolysis of organism complexing agent with the inhibition titanium, and adds strong acid to increase the stability of sol system, and cost is higher.The present invention with the fixation support of cross-linking starch microballoon as wastewater treatment catalyst, thereby is nano-TiO after preparing the cross-linking starch microballoon with cheap starch 2Popularization and application opened up wide prospect.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the synthetic method of the shell starch microsphere that a kind of preparation technology is simple, generated time is short, cost is low is provided.
For achieving the above object, the technical solution used in the present invention is: at first, by mass fraction the titanium dioxide of 0.4-0.6 part, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, the starch solution that N '-methylene-bisacrylamide and second step obtain at 50～60 ℃, reacted 3-4 hour with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 55～65 ℃ vacuum dryings.
Because spherex has good biologically active and thereby bioaffinity has guaranteed nano-TiO 2Activity, bin stability, spherex also can keep good dispersiveness in water, deposition velocity is fast, and spherex also possesses certain adsorption capacity to the bacterium in the water body, microorganism, utilizes the nano-TiO that carries after the absorption 2The sterilization ability can be carried out double purification to water body.
Embodiment
Embodiment 1: at first, by mass fraction 0.4 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 50 ℃, reacted 4 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 65 ℃ vacuum dryings.
Embodiment 2: at first, by mass fraction 0.6 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 60 ℃, reacted 3 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 55 ℃ vacuum dryings.
Embodiment 3: at first, by mass fraction 0.5 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 55 ℃, reacted 3.5 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 60 ℃ vacuum dryings.
It is long to the invention solves the spherex generated time, the problem that cost is high.Not only particle diameter is less for the hud typed microballoon of institute's synthetic, the particle size range narrowly distributing, and generated time is short, and cost is low.Give core-shell particles with conduction, heat conduction and magnetic function by physical chemistry means (crosslinked, embedding etc.), the Application Areas of spherex fully is expanded, not only can also can be used as perfume compound as the carrier of medicine, sanitary material, paper strengthening agent and filler, sewage disposal etc.

Claims (4)

1, a kind of synthetic method of shell starch microsphere is characterized in that:
1) at first, the titanium dioxide of 0.4-0.6 part, 0.004 part water glass and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO by mass fraction 2Gel;
2) secondly, get 4.5 parts Zulkovsky starch and deionized water by 1: 8 quality than furnishing starch solution;
3) then, press mass fraction, in mixture, dropwise add the TiO of 10% volume again 120 parts hexanaphthene, 1.2 parts initiator, 2.8 parts emulsifier for mixing thorough mixing 2Behind the gel, add 1.2 parts linking agent N again, the starch solution that the N '-methylene-bisacrylamide and second step obtain at 50～60 ℃, reacted 3-4 hour with the stirring velocity of 600r/min;
Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1;
4) last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the throw out that obtains is used ethyl acetate, acetone, dehydrated alcohol thorough washing successively, obtains white to yellowish product, gets final product at 55～65 ℃ vacuum dryings.
2, the synthetic method of shell starch microsphere according to claim 1 is characterized in that: at first, by mass fraction 0.4 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 50 ℃, reacted 4 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 65 ℃ vacuum dryings.
3, the synthetic method of shell starch microsphere according to claim 1 is characterized in that: at first, by mass fraction 0.6 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 60 ℃, reacted 3 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 55 ℃ vacuum dryings.
4, the synthetic method of shell starch microsphere according to claim 1 is characterized in that: at first, by mass fraction 0.5 part titanium dioxide, 0.004 part sodium metasilicate and 33 parts deionized water are carried out sufficient microwave dispersion, obtain TiO 2Gel; Secondly, get 4.5 parts soluble starch and deionized water by 1: 8 quality than furnishing starch solution; Then, by mass fraction 120 parts cyclohexane, 1.2 parts initator, 2.8 parts emulsifier for mixing are fully mixed, in mixture, dropwise add again the TiO of 10% volume 2Behind the gel, add 1.2 parts crosslinking agent N, N '-methylene-bisacrylamide and starch solution at 55 ℃, reacted 3.5 hours with the mixing speed of 600r/min again; Said initator is K 2S 2O 8With NaHSO 3Mixture, K wherein 2S 2O 8With NaHSO 3Mass ratio is 1: 1; Said emulsifying agent is the mixture of Span60 and Tween60, and wherein the mass ratio of Span60 and Tween60 is 2: 1; At last, stop to stir, 2h is left standstill in cooling, and oil phase is removed in centrifugation, and the sediment that obtains is fully washed with ethyl acetate, acetone, absolute ethyl alcohol successively, obtains white to yellowish product, gets final product at 60 ℃ vacuum dryings.
CNB2007100177641A 2007-04-28 2007-04-28 Synthesis method of shell starch microsphere Expired - Fee Related CN100462391C (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
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CN101880348A (en) * 2010-07-20 2010-11-10 季生象 Preparation method for functionalized crosslinked polymer resin microspheres
CN101210080B (en) * 2007-12-21 2010-11-17 陕西科技大学 Method for preparing original starch enhancement modifier
CN102008926A (en) * 2010-11-16 2011-04-13 合肥市君科合成材料有限公司 Method for preparing starch microspheres
CN102249401A (en) * 2011-04-06 2011-11-23 长安大学 Preparation method of multipurpose compound photocatalytic biological cell vector
CN102372785A (en) * 2010-08-07 2012-03-14 江苏天麟生物医药科技有限公司 Simple and feasible method for synthesis of modified starch microspheres in microemulsion system
CN104971047A (en) * 2015-06-16 2015-10-14 浙江中医药大学 Nasal gastrodin pharmacia with biological adhesion characteristic, and preparation method thereof
CN109516614A (en) * 2018-11-23 2019-03-26 宁波欣辉环保科技有限公司 A kind of electroplating wastewater oxidation processing technique of reverse osmosis membrane processing complex compound
CN111729625A (en) * 2020-06-15 2020-10-02 宁波锋成先进能源材料研究院 Nano composite micro-rubber ball and preparation method and application thereof

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CN102949971B (en) * 2012-10-30 2014-09-10 中科院广州化学有限公司 Starch base silica composite microspheres, preparation method and applications thereof

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CN1233699C (en) * 2002-11-22 2005-12-28 陕西科技大学 Method for synthesizing starch microsphere
DE10344660A1 (en) * 2003-09-25 2005-04-28 Merck Patent Gmbh Encapsulated pigments

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101210080B (en) * 2007-12-21 2010-11-17 陕西科技大学 Method for preparing original starch enhancement modifier
CN101880348A (en) * 2010-07-20 2010-11-10 季生象 Preparation method for functionalized crosslinked polymer resin microspheres
CN102372785A (en) * 2010-08-07 2012-03-14 江苏天麟生物医药科技有限公司 Simple and feasible method for synthesis of modified starch microspheres in microemulsion system
CN102008926A (en) * 2010-11-16 2011-04-13 合肥市君科合成材料有限公司 Method for preparing starch microspheres
CN102008926B (en) * 2010-11-16 2013-01-09 合肥市君科合成材料有限公司 Method for preparing starch microspheres
CN102249401A (en) * 2011-04-06 2011-11-23 长安大学 Preparation method of multipurpose compound photocatalytic biological cell vector
CN102249401B (en) * 2011-04-06 2012-09-26 长安大学 Preparation method of multipurpose compound photocatalytic biological cell vector
CN104971047A (en) * 2015-06-16 2015-10-14 浙江中医药大学 Nasal gastrodin pharmacia with biological adhesion characteristic, and preparation method thereof
CN104971047B (en) * 2015-06-16 2017-09-26 浙江中医药大学 Gastrodine nosal spherex with bio-adhesive characteristic and preparation method thereof
CN109516614A (en) * 2018-11-23 2019-03-26 宁波欣辉环保科技有限公司 A kind of electroplating wastewater oxidation processing technique of reverse osmosis membrane processing complex compound
CN111729625A (en) * 2020-06-15 2020-10-02 宁波锋成先进能源材料研究院 Nano composite micro-rubber ball and preparation method and application thereof

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