CN111234040A - 一种尿素改性淀粉的制备方法及其应用 - Google Patents
一种尿素改性淀粉的制备方法及其应用 Download PDFInfo
- Publication number
- CN111234040A CN111234040A CN202010021245.8A CN202010021245A CN111234040A CN 111234040 A CN111234040 A CN 111234040A CN 202010021245 A CN202010021245 A CN 202010021245A CN 111234040 A CN111234040 A CN 111234040A
- Authority
- CN
- China
- Prior art keywords
- starch
- urea
- modified starch
- preparation
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000004202 carbamide Substances 0.000 title claims abstract description 56
- 229920000881 Modified starch Polymers 0.000 title claims abstract description 53
- 239000004368 Modified starch Substances 0.000 title claims abstract description 53
- 235000019426 modified starch Nutrition 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920002472 Starch Polymers 0.000 claims abstract description 68
- 235000019698 starch Nutrition 0.000 claims abstract description 65
- 239000008107 starch Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000004108 freeze drying Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 229920001592 potato starch Polymers 0.000 claims description 6
- 229920002261 Corn starch Polymers 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000008120 corn starch Substances 0.000 claims description 5
- 235000003283 Pachira macrocarpa Nutrition 0.000 claims description 4
- 240000001085 Trapa natans Species 0.000 claims description 4
- 235000014364 Trapa natans Nutrition 0.000 claims description 4
- 235000009165 saligot Nutrition 0.000 claims description 4
- 244000017020 Ipomoea batatas Species 0.000 claims description 3
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 3
- 240000003183 Manihot esculenta Species 0.000 claims description 3
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 3
- 240000002853 Nelumbo nucifera Species 0.000 claims description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 3
- 239000011358 absorbing material Substances 0.000 claims description 3
- 235000013373 food additive Nutrition 0.000 claims description 3
- 239000002778 food additive Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229940100445 wheat starch Drugs 0.000 claims description 3
- 240000004922 Vigna radiata Species 0.000 claims description 2
- 235000010721 Vigna radiata var radiata Nutrition 0.000 claims description 2
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 claims description 2
- 239000008394 flocculating agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 11
- 230000004048 modification Effects 0.000 abstract description 11
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 7
- 238000001212 derivatisation Methods 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 2
- 239000008108 microcrystalline cellulose Substances 0.000 description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000003086 food stabiliser Nutrition 0.000 description 1
- 235000003132 food thickener Nutrition 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/212—Starch; Modified starch; Starch derivatives, e.g. esters or ethers
- A23L29/219—Chemically modified starch; Reaction or complexation products of starch with other chemicals
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/04—Starch derivatives, e.g. crosslinked derivatives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
- C09J103/04—Starch derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Water Supply & Treatment (AREA)
- Animal Behavior & Ethology (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Dispersion Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Molecular Biology (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicinal Preparation (AREA)
Abstract
本发明公开了一种尿素改性淀粉的制备方法及其应用,包括如下步骤:(1)将尿素、水和淀粉混合搅拌均匀,经过滤后冷冻干燥;(2)将步骤(1)所得的物料进行粉碎,于50‑150℃保温反应1‑50h,或于50‑1200W的功率下进行微波辐照加热10s‑60min,冷却至室温;(3)将步骤(2)所得的物料经充分水洗,再进行真空干燥,即得所述尿素改性淀粉,其含氮量为0.01‑15wt%。本发明在无溶剂无催化剂条件下用尿素对淀粉进行改性,工艺简便、绿色环保、能耗低,不仅减少了普通淀粉改性的复杂步骤,也克服了已有法的耗时长、条件苛刻、成本高、后处理复杂,且副产品较多的问题。
Description
技术领域
本发明属于淀粉改性技术领域,具体涉及一种尿素改性淀粉的制备方法及其应用。
背景技术
淀粉存在于许多植物的种子、茎或块根中,来源丰富、价格低廉、安全无毒,是一种可再生、可生物降解、良好生物相容性的天然高分子,是人类和其它生物所需的碳源、能量的重要来源。淀粉的基本构成单位为葡萄糖,葡萄糖脱去水分子后经由糖苷键连结在一起所形成的聚合物。淀粉具有优点,淀粉中含有大量的羟基,可通过衍生化改性获得功能材料,或者也可通过水解获得醇、醛、酮、酸、酯、醚等产物,因此也是重要的化工原料。因此,对于淀粉的研究、高值化开发利用,符合环境保护和可持续发展战略。
淀粉在植物中一般呈粒状,不同来源的淀粉颗粒的大小相差很大,一般介于3~120μm之间。淀粉分子中含有大量的羟基,会形成分子内和分子间氢键,促使淀粉分子结晶。因而淀粉具有半结晶的性质,即淀粉颗粒内部存在着两种不同的结构--结晶结构和无定形结构。淀粉的半结晶的性质导致其难以溶解于普通溶剂中,造成其加工、改性难度增加。把淀粉分散在水中,搅拌制成淀粉乳,并对体系进行缓慢加热,直至温度高于80℃,可获得糊化淀粉。糊化淀粉体系粘度高,具有较好的粘合、凝胶、成膜等性能,可广泛应用于食品、医药、化工、造纸、纺织等行业中。然而,正是由于糊化淀后粘度提高,导致其均匀化升温过程难度大、耗时长、产品性能不稳定,并且消耗大量能源。因此,对淀粉的衍生化改性开发利用十分必要。例如,Q.Xu等(BioResources,2016,11(3),6756-6767)在水介质中将醋酸乙烯酯和丙烯酸丁酯接枝到淀粉分子上,获得粘度低、玻璃化温度低的改性淀粉,提升了淀粉作为粘合剂的应用性能。值得提及的是,糊化淀粉在浓度较高时虽然外观较均匀,但低浓度时仍可观察到淀粉在水中分散不均匀、易于沉降,从而降低淀粉应有的效能。H.Yang等(WaterResearch,2017,118 160-166)以过硫酸钾为引发剂,在N2气氛下将丙烯酰胺和甲基丙烯酰氧乙基三甲基氯化铵加入在糊化淀粉中,经水浴55℃加热后,制得在水中具有良好分散性的改性淀粉,表现出优异的絮凝性能。然而,反应介质水的存在,使得淀粉改性需要的更多能源,并且大量污染水需要后处理,导致成本大大提升。由此,需开发无溶剂介质的淀粉衍生化改性方法。Y.Wu等(Polymers,2019,11,72)将淀粉和马来酸酐或者乳酸或者丙烯酸甲酯在无溶剂下直接混合,采用常规加热方式制得了接枝率较低的淀粉衍生化改性产物;尽管接枝率低,所得改性淀粉的水分散性、粘度等性能却获得大大改善。这些研究结果说明,淀粉分子中的大量羟基是能够衍生化改性,同时说明衍生化改性程度强烈影响淀粉的功能和性能。
近年来,虽然微波辐照辅助化学反应的确切原理仍有较大争议,但其对能源的高效利用、辅助化学反应的高效和快速,使微波辅辐照助技术在化学合成、热处理等领域受到越来越多的关注,逐渐成为热点。例如,X.Xiong等(ACS Sustainable Chem.Eng.2018,6(9):12320-12327;Carbohydr.Polym.2018,201:367-373)采用微波辐照加热的方式,在无任何外加催化剂、引发剂以及化学反应介质条件下,成功地对微晶纤维素粉末进行了氨基甲酸酯化或者聚丙烯酰胺化的表面改性,大大提升了微晶纤维素的水分散性和悬浮稳定性。据报道(Starch 1981,33,84-90),尿素分子能成为氢键中H原子供给体,从而有助于淀粉在常温下的糊化,获得二者在分子水平的混合物体系。由此,将常温下的尿素糊化淀粉体系脱水后,进行无溶剂、无催化剂条件下进行加热,可望成为低污染、高安全性地进行淀粉改性的新方法。
发明内容
本发明的目的在于克服现有技术缺陷,提供一种尿素改性淀粉的制备方法。
本发明的另一目的在于提供上述尿素改性淀粉的应用。
本发明的技术方案如下:
一种尿素改性淀粉的制备方法,包括如下步骤:
(1)将尿素、水和淀粉混合搅拌均匀,经过滤后冷冻干燥;
(2)将步骤(1)所得的物料进行粉碎,于50-150℃保温反应1-50h,或于50-1200W的功率下进行微波辐照加热10s-60min,冷却至室温;
(3)将步骤(2)所得的物料经充分水洗,再进行真空干燥,即得所述尿素改性淀粉,其含氮量为0.01-15wt%。
在本发明的一个优选实施方案中,所述保温反应的温度为50-120℃,时间为2-48h。
在本发明的一个优选实施方案中,所述微波辐照加热的功率为120-1000W,时间为30s-20min。
在本发明的一个优选实施方案中,所述淀粉包括玉米淀粉、马铃薯淀粉、小麦淀粉、菱角淀粉、莲藕淀粉、荸荠淀粉、绿豆淀粉、甘薯淀粉和木薯淀粉中的至少一种。
在本发明的一个优选实施方案中,所述尿素、水和淀粉的质量比为5-30∶25-35∶4-6。
上述制备方法制备的尿素改性淀粉在制备生物医用材料中的应用。
上述制备方法制备的尿素改性淀粉在制备食品添加剂中的应用。该食品添加剂优选为食品增稠剂或食品稳定剂。
上述制备方法制备的尿素改性淀粉在制备絮凝剂中的应用。
上述制备方法制备的尿素改性淀粉在制备吸水材料中的应用。
上述制备方法制备的尿素改性淀粉在制备粘合剂组合物中的应用。
本发明的有益效果是:
1、本发明在无溶剂无催化剂条件下用尿素对淀粉进行改性,工艺简便、绿色环保、能耗低,不仅减少了普通淀粉改性的复杂步骤,也克服了已有法的耗时长、条件苛刻、成本高、后处理复杂,且副产品较多的问题。
2、本发明所制得的尿素改性淀粉,水分散性和悬浮性能有较大的提升,在医药辅料、食品增稠或稳定剂、絮凝剂、吸水材料、粘合剂或粘合剂辅料以及用于制备生物医用材料等方面有着广阔的应用前景。
附图说明
图1为本发明实施例1制得的尿素改性淀粉的扫描电镜照片。
图2为本发明实施例2制得的尿素改性淀粉的扫描电镜照片。
图3为本发明实施例3制得的尿素改性淀粉的扫描电镜照片。
图4为本发明实施例4制得的尿素改性淀粉与原淀粉原料的傅里叶红外光谱对照图。
图5为本发明实施例5制得的尿素改性淀粉的氮含量随尿素与淀粉质量比的变化曲线图。
图6为本发明实施例6制得的尿素改性淀粉的分散和悬浮状态照片。
图7为本发明实施例7的实验结果图。
具体实施方式
以下通过具体实施方式结合附图对本发明的技术方案进行进一步的说明和描述。
实施例1
准确称取尿素10g,并加入30g的水,再加入5g玉米淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行油浴加热至65℃并保温48h。产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,在扫描电镜下观察如图1所示,并经元素分析仪测试氮含量为0.07%。
实施例2
准确称取尿素10g,并加入30g的水,再加入5g玉米淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行微波辐照加热,微波功率为240W、微波辐照加热时间为1min;产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,在扫描电镜下观察如图2所示,并经元素分析仪测试氮含量为1.26%。
实施例3
准确称取尿素15g,并加入30g的水,再加入5g马铃薯淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行微波辐照加热,微波功率为780W、微波辐照加热时间为3min;产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,在扫描电镜下观察如图3所示,并经元素分析仪测试氮含量为6.31%。
实施例4
准确称取尿素15g,并加入30g的水,再加入5g木薯淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行油浴加热至50℃并保温24h。产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,并经元素分析仪测试氮含量为0.45%,其与原淀粉原料的红外光谱对照如图4所示,其中1719cm-1处的红外吸收证明淀粉氨基甲酸酯化成功。
实施例5
分别准确称取尿素5g、10g、20g、30g,并各自加入30g的水和5g小麦淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行微波辐照加热,微波功率为616W、微波辐照加热时间为4min;产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,并经元素分析仪测试氮含量,所得尿素改性淀粉氮含量随尿素与淀粉质量比的变化如图5所示。
实施例6
准确称取尿素5g,并加入30g的水,再加入5g甘薯淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行微波辐照加热,微波功率为800W、微波辐照加热时间为5min;产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,并经元素分析仪测试氮含量为2.94%。将所得尿素改性淀粉加入质量分数为2%的壳聚糖溶液中,添加量分别为总质量的1%、2.5%和5%,经搅拌1h、静置5h,可观察到本实施例制得的尿素改性淀粉能均匀分散和悬浮,未见沉降(照片参见图6)。
实施例7
分别配制质量分数均为15%的聚乙烯醇(PVA)溶液、未改性淀粉悬浮浆、实施例3所得尿素改性淀粉悬浮浆,将聚乙烯醇溶液和尿素改性淀粉悬浮浆等质量混合;将上述溶液或浆料采用国标方法测试其粘结强度,图7显示尿素改性淀粉能显著提升PVA的粘结强度。
实施例8
准确称取尿素10g,并加入30g的水,再加入5g莲藕淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行油浴加热至50℃并保温1h,或者于120℃并保温48h。产物分别经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,经元素分析仪测试氮含量分别为0.02%和0.19%。
实施例9
准确称取尿素10g,并加入30g的水,再加入5g玉米淀粉,搅拌约1h后过滤再于-40℃冷冻干燥48h;取出干燥物粉碎,置于烧瓶中进行微波辐照加热,微波功率为120W、微波辐照加热时间为30s,或者微波功率为1000W、微波辐照加热时间为30s,或者微波功率为360W、微波辐照加热时间为20min;所得产物经降温至室温,水洗三次,再通过真空干燥后,制得所述尿素改性淀粉,本实施例制得的尿素改性淀粉经元素分析仪测试氮含量分别为0.24%、2.89%和13.9%。
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (10)
1.一种尿素改性淀粉的制备方法,其特征在于:包括如下步骤:
(1)将尿素、水和淀粉混合搅拌均匀,经过滤后冷冻干燥;
(2)将步骤(1)所得的物料进行粉碎,于50-150℃保温反应1-50h,或于50-1200W的功率下进行微波辐照加热10s-60min,冷却至室温;
(3)将步骤(2)所得的物料经充分水洗,再进行真空干燥,即得所述尿素改性淀粉,其含氮量为0.01-15wt%。
2.如权利要求1所述的制备方法,其特征在于:所述保温反应的温度为50-120℃,时间为2-48h。
3.如权利要求1所述的制备方法,其特征在于:所述微波辐照加热的功率为120-1000W,时间为30s-20min。
4.如权利要求1所述的制备方法,其特征在于:所述淀粉包括玉米淀粉、马铃薯淀粉、小麦淀粉、菱角淀粉、莲藕淀粉、荸荠淀粉、绿豆淀粉、甘薯淀粉和木薯淀粉中的至少一种。
5.如权利要求1至4中任一权利要求所述的制备方法,其特征在于:所述尿素、水和淀粉的质量比为5-30∶25-35∶4-6。
6.权利要求1至5中任一权利要求所述的制备方法制备的尿素改性淀粉在制备生物医用材料中的应用。
7.权利要求1至5中任一权利要求所述的制备方法制备的尿素改性淀粉在制备食品添加剂中的应用。
8.权利要求1至5中任一权利要求所述的制备方法制备的尿素改性淀粉在制备絮凝剂中的应用。
9.权利要求1至5中任一权利要求所述的制备方法制备的尿素改性淀粉在制备吸水材料中的应用。
10.权利要求1至5中任一权利要求所述的制备方法制备的尿素改性淀粉在制备粘合剂组合物中的应用。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010021245.8A CN111234040A (zh) | 2020-01-09 | 2020-01-09 | 一种尿素改性淀粉的制备方法及其应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010021245.8A CN111234040A (zh) | 2020-01-09 | 2020-01-09 | 一种尿素改性淀粉的制备方法及其应用 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111234040A true CN111234040A (zh) | 2020-06-05 |
Family
ID=70862938
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010021245.8A Pending CN111234040A (zh) | 2020-01-09 | 2020-01-09 | 一种尿素改性淀粉的制备方法及其应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111234040A (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112724524A (zh) * | 2020-12-28 | 2021-04-30 | 会通新材料股份有限公司 | 一种可生物降解阻燃聚丙烯复合材料及其制备方法 |
CN113563845A (zh) * | 2021-08-18 | 2021-10-29 | 山西和合众新材料科技有限公司 | 一种绿色环保可降解固尘剂及其制备方法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1425624A (en) * | 1973-08-10 | 1976-02-18 | Scholten Honig Research Bfv | Chemical modification of starches |
CN103790038A (zh) * | 2014-01-17 | 2014-05-14 | 郝军元 | 以淀粉为原料制备活性印花糊料的方法 |
CN105670191A (zh) * | 2016-04-21 | 2016-06-15 | 广东石油化工学院 | 一种改性淀粉-聚乙烯醇可降解薄膜专用料 |
-
2020
- 2020-01-09 CN CN202010021245.8A patent/CN111234040A/zh active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1425624A (en) * | 1973-08-10 | 1976-02-18 | Scholten Honig Research Bfv | Chemical modification of starches |
CN103790038A (zh) * | 2014-01-17 | 2014-05-14 | 郝军元 | 以淀粉为原料制备活性印花糊料的方法 |
CN105670191A (zh) * | 2016-04-21 | 2016-06-15 | 广东石油化工学院 | 一种改性淀粉-聚乙烯醇可降解薄膜专用料 |
Non-Patent Citations (6)
Title |
---|
PRZEMYSLAW SIEMION ET AL.: ""Solid State Reactions of Potato Starch with Urea and Biuret"", 《JOURNAL OF POLYMERS AND THE ENVIRONMENT》 * |
SIKORA MAREK ET AL.: ""Chemical starch modification in the field of microwaves. II. Reaction of potato starch with carboxyamides and carboxylic esters"", 《POLISH JOURNAL OF FOOD AND NUTRITION SCIENCES》 * |
唐双凌等: ""氨基甲酸淀粉酯的改进合成及其性能研究"", 《化工新型材料》 * |
李跃华等: ""氨基甲酸酯变性淀粉对淀粉/PVA混合浆相分离的影响"", 《印染助剂》 * |
王薇青等译,[日]二国二郎主编: "《淀粉科学手册(第1版)》", 31 October 1990, 轻工业出版社 * |
郭磊: ""氨基甲酸酯系淀粉衍生物的合成与应用"", 《中国优秀博硕士学位论文全文数据库(博士)工程科技I辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112724524A (zh) * | 2020-12-28 | 2021-04-30 | 会通新材料股份有限公司 | 一种可生物降解阻燃聚丙烯复合材料及其制备方法 |
CN112724524B (zh) * | 2020-12-28 | 2022-04-01 | 会通新材料股份有限公司 | 一种可生物降解阻燃聚丙烯复合材料及其制备方法 |
CN113563845A (zh) * | 2021-08-18 | 2021-10-29 | 山西和合众新材料科技有限公司 | 一种绿色环保可降解固尘剂及其制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Zuo et al. | Preparation and characterization of dialdehyde starch by one-step acid hydrolysis and oxidation | |
Rajan et al. | Enzymatic modification of cassava starch by fungal lipase | |
Adak et al. | A green approach for starch modification: Esterification by lipase and novel imidazolium surfactant | |
KR100378241B1 (ko) | 초흡수제및이의제조방법 | |
Borzacchiello et al. | Chitosan-based hydrogels: synthesis and characterization | |
CN108164903B (zh) | 一种聚天冬氨酸半互穿纳米复合水凝胶及其制备工艺 | |
CN104164199A (zh) | 一种淀粉基生物质功能胶粘剂及其制备方法 | |
CN111234040A (zh) | 一种尿素改性淀粉的制备方法及其应用 | |
CN101200393A (zh) | 一种用于生产包膜肥料的膜材料及其制备工艺 | |
CN108659171B (zh) | 一种纳米纤维素超强吸水树脂的制备方法 | |
WO2017020237A1 (zh) | 三重响应型淀粉基微凝胶及其制备方法 | |
CN102399841A (zh) | 一种淀粉醋酸酯的合成方法 | |
Yılmaz et al. | Effect of ultrasound-microwave and microwave-ultrasound treatment on physicochemical properties of corn starch | |
CN103254449A (zh) | 一种醋酸酯淀粉的制备方法 | |
CN111875230A (zh) | 全生物质絮凝剂及其制备方法 | |
Liu et al. | Study on the structure and physicochemical properties of fenugreek galactomannan modified via octenyl succinic anhydride | |
CN111333990A (zh) | 一种自修复型双网络交联可降解丙烯酸水凝胶及其制法 | |
CN108383945B (zh) | 一种农用保水剂及其制备方法 | |
CN111303305A (zh) | 一种电场耦合超声制备高取代度乙酰化淀粉的方法 | |
CN107573422B (zh) | 辛烯基琥珀酸淀粉酯的制备方法 | |
CN103214587A (zh) | 一种应用超声波技术加工复合变性淀粉的方法 | |
JPH06233691A (ja) | バクテリアセルロースのキセロゲルの製法及びそれにより 製造された誘導体 | |
CN114437524B (zh) | 一种甘蔗纤维素基可降解复合材料的制备方法 | |
Sagar et al. | Microwave assisted synthesis of carboxymethyl starch | |
CN1392168A (zh) | 一种高吸水树脂的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200605 |