CN106866830A - A kind of method for improving Arabic gum emulsifiability - Google Patents
A kind of method for improving Arabic gum emulsifiability Download PDFInfo
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- 235000010489 acacia gum Nutrition 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000001785 acacia senegal l. willd gum Substances 0.000 title claims 6
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 claims abstract description 16
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005886 esterification reaction Methods 0.000 claims abstract description 9
- 238000001694 spray drying Methods 0.000 claims abstract description 9
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical group CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 claims abstract 7
- 239000000243 solution Substances 0.000 claims description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 230000032050 esterification Effects 0.000 claims description 2
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 230000007306 turnover Effects 0.000 claims 1
- 229920000084 Gum arabic Polymers 0.000 abstract description 64
- 239000000205 acacia gum Substances 0.000 abstract description 64
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 abstract description 17
- 238000004945 emulsification Methods 0.000 abstract description 14
- 238000001035 drying Methods 0.000 abstract description 10
- 230000001804 emulsifying effect Effects 0.000 abstract description 8
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 241000978776 Senegalia senegal Species 0.000 abstract 7
- 239000000839 emulsion Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 230000007774 longterm Effects 0.000 abstract 1
- 239000003094 microcapsule Substances 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 244000215068 Acacia senegal Species 0.000 description 59
- 239000000047 product Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 241000978782 Vachellia seyal Species 0.000 description 6
- 239000012467 final product Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000010979 pH adjustment Methods 0.000 description 4
- 241000894007 species Species 0.000 description 4
- 241000220479 Acacia Species 0.000 description 3
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 235000006491 Acacia senegal Nutrition 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 210000000416 exudates and transudate Anatomy 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
一种提高阿拉伯胶乳化性能的方法,以乳化性能较差的阿拉伯胶为原料,采用酯化反应,终止反应,喷雾干燥,除残留辛烯基琥珀酸酐,恒温恒湿箱‑烘箱储藏、干燥等技术制备高乳化性能的阿拉伯胶。本发明首先采用辛烯基琥珀酸酐‑单甘酯混合物与阿拉伯胶发生酯化反应,辛烯基琥珀酸基团的引入提高阿拉伯胶的乳化性能,单甘酯的存在对其乳化性能有积极影响,且缩短反应时间,降低生产成本;其次采用恒温恒湿箱‑烘箱储藏、干燥阿拉伯胶,物理改性进一步提高其乳化性能。本方法无有害有机溶剂使用,无环境污染,操作安全,大大提高了阿拉伯胶的乳化性能,拓宽了其应用范围。此产品适用于需长期稳定的乳状液,油脂微胶囊等方面。A method for improving the emulsification performance of gum arabic, using gum arabic with poor emulsification performance as raw material, adopting esterification reaction, terminating the reaction, spray drying, removing residual octenyl succinic anhydride, storing and drying in a constant temperature and humidity box-oven, etc. technology to prepare gum arabic with high emulsifying properties. The present invention first adopts octenyl succinic anhydride-monoglyceride mixture to undergo esterification reaction with gum arabic, the introduction of octenyl succinic acid groups improves the emulsification performance of gum arabic, and the presence of monoglyceride has a positive impact on its emulsification performance , and shorten the reaction time, reduce production costs; secondly, use constant temperature and humidity box-oven to store and dry the gum arabic, and further improve its emulsifying performance through physical modification. The method does not use harmful organic solvents, has no environmental pollution, and is safe to operate, greatly improves the emulsifying performance of the gum arabic, and broadens its application range. This product is suitable for long-term stable emulsions, oil microcapsules, etc.
Description
技术领域technical field
本发明涉及一种提高阿拉伯胶乳化性能的方法,属于食品、化妆品、医药等技术领域。The invention relates to a method for improving the emulsification performance of gum arabic, belonging to the technical fields of food, cosmetics, medicine and the like.
背景技术Background technique
阿拉伯胶是来源于豆科金合欢树属的树枝和树干所分泌的胶状渗出物经干燥而成的树胶,可广泛应用于食品、制药、化妆品等行业。但是阿拉伯胶的性质,特别是乳化性很难达到标准化,不同的植物品种、地理及气候差异,采收后处理等都会造成其理化指标的改变。且与通常的蛋白质乳化剂相比,阿拉伯胶的使用浓度要更高才能达到乳化效果。因此,将阿拉伯胶进行改性以提高其应用性能已逐渐成为当今研究的热点。Gum Arabic is a gum derived from the dried colloidal exudate secreted by the branches and trunks of the leguminous Acacia tree. It can be widely used in food, pharmaceutical, cosmetic and other industries. However, the properties of gum arabic, especially the emulsification, are difficult to achieve standardization. Different plant varieties, geographical and climate differences, post-harvest treatment, etc. will cause changes in its physical and chemical indicators. And compared with the usual protein emulsifiers, the concentration of gum arabic must be higher to achieve the emulsification effect. Therefore, modifying gum arabic to improve its application performance has gradually become a research hotspot.
目前,商业化的阿拉伯胶主要来源于金合欢属的Gemmiferace系和Vulgares系树种,其中Acacia senegal和Acacia seyal是金合欢属植物中被用于采集阿拉伯胶最多的两类树种。来源于Acacia seyal树种的阿拉伯胶(约占商业阿拉伯胶的1/4)的乳化性能一般低于Acacia senegal 。此外,性能优越的阿拉伯胶资源面临枯竭,真正具有商业价值的产品产量很有限。因此,在保持阿拉伯胶原有优良性质的基础上,提高来源于Acacia seyal树种的阿拉伯胶的乳化性能,降低阿拉伯胶在工业中的使用量具有一定的必要性。At present, the commercialized gum arabic mainly comes from the Gemmiferace and Vulgares species of Acacia, among which Acacia senegal and Acacia seyal are the two species most used to collect gum arabic in Acacia. Gum Arabic derived from the Acacia seyal species (about 1/4 of commercial gum Arabic) generally has lower emulsifying properties than Acacia senegal . In addition, the resources of gum arabic with superior performance are facing depletion, and the output of products with real commercial value is very limited. Therefore, on the basis of maintaining the excellent properties of collagen arabic, it is necessary to improve the emulsifying properties of gum arabic derived from Acacia seyal species and reduce the amount of gum arabic used in industry.
国内外有关阿拉伯胶改性以提高其乳化性能的报道很多,最常见的是物理改性,但其过程常涉及到高温加热,易造成阿拉伯胶褐变、结块、焦化。此外,化学改性也是提高阿拉伯胶乳化性能的一种方法,最常见的是采用辛烯基琥珀酸酐进行改性。但是,辛烯基琥珀酸酐难溶于水,若直接使用会造成反应效率低下;若过量使用,其残留量增加,难以除去,增加生产成本。There are many reports on the modification of gum arabic to improve its emulsification performance at home and abroad. The most common is physical modification, but the process often involves high temperature heating, which can easily cause browning, agglomeration, and coking of gum arabic. In addition, chemical modification is also a method to improve the emulsification performance of gum arabic, the most common one is to use octenyl succinic anhydride for modification. However, octenyl succinic anhydride is insoluble in water, and if used directly, the reaction efficiency will be low; if used in excess, its residual amount will increase, making it difficult to remove and increasing production costs.
发明内容Contents of the invention
本发明的目的是针对现有技术不足,提供一种提高阿拉伯胶乳化性能的方法。The purpose of the present invention is to provide a method for improving the emulsification performance of latex arabic against the deficiencies of the prior art.
本发明的技术方案是:通过化学-物理方法,采用辛烯基琥珀酸酐-单甘酯混合物对阿拉伯胶进行化学改性,通过恒温恒湿箱-烘箱物理改性,从而提高其乳化性能,为阿拉伯胶的改性提供一种新的方法和思路,进而拓宽其应用范围;以阿拉伯胶(来源于Acacia seyal树种)为原料,通过酯化反应,喷雾干燥,除残留辛烯基琥珀酸酐,恒温恒湿箱-烘箱储藏、干燥等技术,改善阿拉伯胶的乳化性能。The technical scheme of the present invention is: through chemical-physical method, adopt octenyl succinic anhydride-monoglyceride mixture to carry out chemical modification to gum arabic, through constant temperature and humidity box-oven physical modification, thereby improve its emulsifying performance, for The modification of gum arabic provides a new method and idea, and then broadens its application scope; using gum arabic (derived from Acacia seyal species) as raw material, through esterification, spray drying, removal of residual octenyl succinic anhydride, constant temperature Constant humidity box-oven storage, drying and other technologies can improve the emulsification performance of gum arabic.
本发明所述方法为:The method of the present invention is:
1、阿拉伯胶溶液制备:称取阿拉伯胶与蒸馏水混合,在50~60 ℃的水浴中搅拌溶解,过滤,配制质量浓度为20%~40%的阿拉伯胶溶液。1. Preparation of gum arabic solution: Mix gum arabic with distilled water, stir and dissolve in a water bath at 50-60 °C, filter, and prepare a gum arabic solution with a mass concentration of 20%-40%.
2、阿拉伯胶溶液pH值调节:采用0.5 mol/L NaOH溶液和0.1 mol/L HCl溶液调节阿拉伯胶溶液的初始pH值至8.0。2. pH adjustment of the gum arabic solution: adjust the initial pH of the gum arabic solution to 8.0 with 0.5 mol/L NaOH solution and 0.1 mol/L HCl solution.
3、辛烯基琥珀酸酐-单甘酯混合物制备:将占阿拉伯胶干基质量的3% 的辛烯基琥珀酸酐和占辛烯基琥珀酸酐质量的10%的单甘酯在60~70 ℃的温度下混合,使单甘酯完全溶解,制备辛烯基琥珀酸酐-单甘酯混合物。3. Preparation of octenyl succinic anhydride-monoglyceride mixture: 3% octenyl succinic anhydride and 10% octenyl succinic anhydride monoglyceride at 60~70 °C Mix at a certain temperature to completely dissolve the monoglyceride to prepare an octenyl succinic anhydride-monoglyceride mixture.
4、酯化反应:将阿拉伯胶溶液放置在磁力搅拌器中搅拌,温度为20~40 ℃条件下,将辛烯基琥珀酸酐-单甘酯混合物缓慢且均匀地加入到阿拉伯胶水溶液中,每滴加一次混合物,采用高速剪切分散机分散30 s,用0.5 mol/L NaOH溶液调节且保持反应液pH值在9.0,重复上述步骤,反应1~2 h后,用0.1 mol/L HCL溶液调节反应液pH值至6.0,终止反应。4. Esterification reaction: place the gum arabic solution in a magnetic stirrer and stir at a temperature of 20-40 °C, slowly and evenly add the mixture of octenyl succinic anhydride-monoglyceride to the aqueous gum arabic solution, every Add the mixture dropwise once, use a high-speed shear disperser to disperse for 30 s, use 0.5 mol/L NaOH solution to adjust and keep the pH value of the reaction solution at 9.0, repeat the above steps, after 1-2 h of reaction, use 0.1 mol/L HCL solution Adjust the pH value of the reaction solution to 6.0 to terminate the reaction.
5、喷雾干燥:将反应终止液在进出风温度分别为180 ℃和90~95 ℃,进样流度为20 r/min的条件下,进行喷雾干燥。5. Spray-drying: Spray-dry the reaction-terminated solution under the conditions that the inlet and outlet air temperatures are 180°C and 90-95°C respectively, and the injection flow rate is 20 r/min.
6、除残留辛烯基琥珀酸酐:采用95%乙醇反复洗涤喷雾干燥得到的产品3~5次,除去残留辛烯基琥珀酸酐后,回收无水乙醇。6. Removal of residual octenyl succinic anhydride: use 95% ethanol to repeatedly wash and spray-dry the product for 3 to 5 times, and recover absolute ethanol after removing residual octenyl succinic anhydride.
7、恒温恒湿箱-烘箱储藏、干燥洗涤后的阿拉伯胶:将洗涤得到的产品放在恒温恒湿箱中,在温度为60 ℃,湿度为75%的条件下储藏12~24 h后,转移到烘箱中,在温度为60℃的条件下干燥2 h后得到最终产品。7. Constant temperature and humidity box-oven storage, drying and washing of gum arabic: put the washed product in a constant temperature and humidity box, and store it at a temperature of 60 °C and a humidity of 75% for 12~24 hours. Transfer to an oven and dry at 60°C for 2 h to obtain the final product.
本产品的特征:本发明以乳化性能比较差的阿拉伯胶(来源于Acacia seyal树种)为原料,通过单甘酯-辛烯基琥珀酸酐和阿拉伯胶酯化反应,喷雾干燥,除残留辛烯基琥珀酸酐,恒温恒湿箱-烘箱储藏、干燥等技术对其进行改性,提高了反应效率,降低了生产成本,确保了产品安全,同时提高了阿拉伯胶的乳化性能,解决了阿拉伯胶乳化性能不稳定的问题。Features of this product: the present invention uses gum arabic (derived from Acacia seyal species) with relatively poor emulsifying properties as raw material, through the esterification reaction of monoglyceride-octenyl succinic anhydride and gum arabic, and spray drying to remove residual octenyl groups. Succinic anhydride is modified by constant temperature and humidity box-oven storage, drying and other technologies, which improves the reaction efficiency, reduces production costs, ensures product safety, and improves the emulsification performance of gum arabic at the same time, solving the problem of gum arabic emulsification performance unstable problem.
本发明的有益效果:以阿拉伯胶(来源于Acacia seyal树种)为原料,结合化学、物理方法对其进行改性,提高了阿拉伯胶的乳化性能,降低了其因树种、树龄、气候等不同造成的乳化性能差异,增加了真正具有商业价值的产品产量,少了其在食品工业中的使用量。同时其应用范围也得到大大拓展。Beneficial effects of the present invention: use gum arabic (derived from Acacia seyal tree species) as raw material, modify it in combination with chemical and physical methods, improve the emulsification performance of gum arabic, and reduce the risk caused by differences in tree species, tree age, climate, etc. The difference in emulsifying properties increases the output of products with real commercial value and reduces its use in the food industry. At the same time, its application range has also been greatly expanded.
具体实施方式detailed description
实施例1Example 1
1、阿拉伯胶溶液制备:称取阿拉伯胶100 g与蒸馏水混合,在55 ℃的水浴中搅拌溶解,过滤,配制质量浓度为20%的阿拉伯胶溶液。1. Preparation of gum arabic solution: weigh 100 g of gum arabic and mix it with distilled water, stir and dissolve in a water bath at 55 °C, filter, and prepare a gum arabic solution with a mass concentration of 20%.
2、阿拉伯胶溶液pH值调节:采用0.5 mol/L NaOH溶液和0.1 mol/L HCl溶液调节阿拉伯胶溶液的初始pH值至8.0。2. pH adjustment of the gum arabic solution: adjust the initial pH of the gum arabic solution to 8.0 with 0.5 mol/L NaOH solution and 0.1 mol/L HCl solution.
3、辛烯基琥珀酸酐-单甘酯混合物制备:将单甘酯(0.3 g)加入到辛烯基琥珀酸酐(3 g)中。在65 ℃的温度下完全溶解单甘酯,制备辛烯基琥珀酸酐-单甘酯混合物。3. Preparation of octenyl succinic anhydride-monoglyceride mixture: Add monoglyceride (0.3 g) to octenyl succinic anhydride (3 g). Completely dissolve monoglyceride at a temperature of 65°C to prepare octenyl succinic anhydride-monoglyceride mixture.
4、酯化反应:将阿拉伯胶溶液放置在磁力搅拌器中搅拌,在温度为20 ℃条件下,将辛烯基琥珀酸酐-单甘酯混合物缓慢且均匀地加入到阿拉伯胶水溶液中,每滴加一次混合物,采用高速剪切分散机分散30 s。用0.5 mol/L NaOH溶液调节且保持反应液pH值在9.0,重复上述步骤。反应1 h后,用0.1 mol/L HCl溶液调节反应液pH值至6.0,终止反应。4. Esterification reaction: place the gum arabic solution in a magnetic stirrer and stir, and at a temperature of 20°C, slowly and evenly add the octenyl succinic anhydride-monoglyceride mixture to the aqueous gum arabic solution, each drop Add the mixture once and disperse for 30 s with a high-speed shear disperser. Use 0.5 mol/L NaOH solution to adjust and keep the pH value of the reaction solution at 9.0, repeat the above steps. After reacting for 1 h, the pH value of the reaction solution was adjusted to 6.0 with 0.1 mol/L HCl solution to terminate the reaction.
5、喷雾干燥:将反应终止液在进出风温度分别为180 ℃、90 ℃,进样流度为20 r/min的条件下,进行喷雾干燥。5. Spray-drying: Spray-dry the reaction-terminated liquid under the condition that the inlet and outlet air temperatures are 180°C and 90°C respectively, and the injection fluidity is 20 r/min.
6、除残留辛烯基琥珀酸酐:采用95%乙醇反复洗涤喷雾干燥得到的产品3次,除去残留辛烯基琥珀酸酐后,回收无水乙醇。6. Removal of residual octenyl succinic anhydride: use 95% ethanol to repeatedly wash and spray-dry the product 3 times, remove residual octenyl succinic anhydride, and recover absolute ethanol.
7、恒温恒湿箱-烘箱储藏、干燥洗涤后的阿拉伯胶:将洗涤得到的产品放置在温度为60 ℃,湿度为75%恒温恒湿箱中,储藏12 h;然后转移到温度为60 ℃的烘箱中,干燥2 h后得到最终产品。7. Constant temperature and humidity box-oven storage and drying of gum arabic after washing: place the washed product in a constant temperature and humidity box with a temperature of 60 °C and a humidity of 75% for 12 hours; then transfer to a temperature of 60 °C The final product was obtained after drying in an oven for 2 h.
实施例2Example 2
1、阿拉伯胶溶液制备:称取阿拉伯胶100 g与蒸馏水混合,在60 ℃的水浴中搅拌溶解,过滤,配制质量浓度为30%的阿拉伯胶溶液。1. Preparation of gum arabic solution: weigh 100 g of gum arabic and mix it with distilled water, stir and dissolve in a water bath at 60 °C, filter, and prepare a gum arabic solution with a mass concentration of 30%.
2、阿拉伯胶溶液pH值调节:采用0.5 mol/L NaOH溶液和0.1 mol/L HCl溶液调节阿拉伯胶溶液的初始pH值至8.0。2. pH adjustment of the gum arabic solution: adjust the initial pH of the gum arabic solution to 8.0 with 0.5 mol/L NaOH solution and 0.1 mol/L HCl solution.
3、辛烯基琥珀酸酐-单甘酯混合物制备:将单甘酯(0.3 g)加入到辛烯基琥珀酸酐(3 g)中,在65 ℃的温度下完全溶解单甘酯,制备辛烯基琥珀酸酐-单甘酯混合物。3. Preparation of octenyl succinic anhydride-monoglyceride mixture: Add monoglyceride (0.3 g) to octenyl succinic anhydride (3 g), and completely dissolve the monoglyceride at a temperature of 65 °C to prepare octenyl Succinic anhydride-monoglyceride mixture.
4、酯化反应:将阿拉伯胶溶液放置在磁力搅拌器中搅拌,在温度为30 ℃条件下,将辛烯基琥珀酸酐-单甘酯混合物缓慢且均匀地加入到阿拉伯胶水溶液中,每滴加一次混合物,采用高速剪切分散机分散30 s。用0.5 mol/L NaOH溶液调节且保持反应液pH值在9.0,重复上述步骤。反应1.5 h后,用0.1 mol/L HCl溶液调节反应液pH值至6.0,终止反应。4. Esterification reaction: place the gum arabic solution in a magnetic stirrer and stir, and at a temperature of 30 °C, slowly and evenly add the mixture of octenyl succinic anhydride-monoglyceride to the aqueous gum arabic solution, each drop Add the mixture once and disperse for 30 s with a high-speed shear disperser. Use 0.5 mol/L NaOH solution to adjust and keep the pH value of the reaction solution at 9.0, repeat the above steps. After reacting for 1.5 h, the pH value of the reaction solution was adjusted to 6.0 with 0.1 mol/L HCl solution to terminate the reaction.
5、喷雾干燥:将反应终止液在进出风温度分别为180 ℃、90 ℃,进样流度为20 r/min的条件下,进行喷雾干燥。5. Spray-drying: Spray-dry the reaction-terminated liquid under the condition that the inlet and outlet air temperatures are 180°C and 90°C respectively, and the injection fluidity is 20 r/min.
6、除残留辛烯基琥珀酸酐:采用95%乙醇反复洗涤喷雾干燥得到的产品4次,除去残留辛烯基琥珀酸酐后,回收无水乙醇。6. Removal of residual octenyl succinic anhydride: use 95% ethanol to repeatedly wash and spray-dry the product 4 times, remove residual octenyl succinic anhydride, and recover anhydrous ethanol.
7、恒温恒湿箱-烘箱储藏、干燥洗涤后的阿拉伯胶:将洗涤得到的产品放置在温度为60 ℃,湿度为75%恒温恒湿箱中,储藏24 h;然后转移到温度为60 ℃的烘箱中,干燥2 h后得到最终产品。7. Constant temperature and humidity box-oven storage and drying of the washed gum arabic: place the washed product in a constant temperature and humidity box with a temperature of 60 °C and a humidity of 75% for 24 hours; then transfer to a temperature of 60 °C The final product was obtained after drying in an oven for 2 h.
实施例3Example 3
1、阿拉伯胶溶液制备:称阿拉伯胶100 g与蒸馏水混合,在60 ℃的水浴中搅拌溶解,过滤,配制质量浓度为40%的阿拉伯胶溶液。1. Preparation of gum arabic solution: Mix 100 g of gum arabic with distilled water, stir and dissolve in a water bath at 60 °C, filter, and prepare a gum arabic solution with a mass concentration of 40%.
2、阿拉伯胶溶液pH值调节:采用0.5 mol/L NaOH溶液和0.1 mol/L HCl溶液调节阿拉伯胶溶液的初始pH值至8.0。2. pH adjustment of the gum arabic solution: adjust the initial pH of the gum arabic solution to 8.0 with 0.5 mol/L NaOH solution and 0.1 mol/L HCl solution.
3、辛烯基琥珀酸酐-单甘酯混合物制备:将单甘酯(0.3 g)加入到辛烯基琥珀酸酐(3 g)中,在65 ℃的温度下完全溶解单甘酯,制备辛烯基琥珀酸酐-单甘酯混合物。3. Preparation of octenyl succinic anhydride-monoglyceride mixture: Add monoglyceride (0.3 g) to octenyl succinic anhydride (3 g), and completely dissolve the monoglyceride at a temperature of 65 °C to prepare octenyl Succinic anhydride-monoglyceride mixture.
4、酯化反应:将阿拉伯胶溶液放置在磁力搅拌器中搅拌,在温度为40 ℃条件下,将辛烯基琥珀酸酐-单甘酯混合物缓慢且均匀地加入到阿拉伯胶水溶液中,每滴加一次混合物,采用高速剪切分散机分散30 s。用0.5 mol/L NaOH溶液调节且保持反应液pH值在9.0,重复上述步骤。反应2 h后,用0.1 mol/L HCl溶液调节反应液pH值至6.0,终止反应。4. Esterification reaction: place the gum arabic solution in a magnetic stirrer and stir, and at a temperature of 40 °C, slowly and evenly add the octenyl succinic anhydride-monoglyceride mixture to the aqueous gum arabic solution, each drop Add the mixture once and disperse for 30 s with a high-speed shear disperser. Use 0.5 mol/L NaOH solution to adjust and keep the pH value of the reaction solution at 9.0, repeat the above steps. After 2 h of reaction, the pH value of the reaction solution was adjusted to 6.0 with 0.1 mol/L HCl solution to terminate the reaction.
5、喷雾干燥:将反应终止液在进出风温度分别为180 ℃、90 ℃,进样流度为20 r/min的条件下,进行喷雾干燥。5. Spray-drying: Spray-dry the reaction-terminated liquid under the condition that the inlet and outlet air temperatures are 180°C and 90°C respectively, and the injection fluidity is 20 r/min.
6、除残留辛烯基琥珀酸酐:采用95%乙醇反复洗涤喷雾干燥得到的产品5次,除去残留辛烯基琥珀酸酐后,回收无水乙醇。6. Removal of residual octenyl succinic anhydride: use 95% ethanol to repeatedly wash and spray-dry the product 5 times, remove residual octenyl succinic anhydride, and recover absolute ethanol.
7、恒温恒湿箱-烘箱储藏、干燥洗涤后的阿拉伯胶:将洗涤得到的产品放置在温度为60 ℃,湿度为75%恒温恒湿箱中,储藏24 h;然后转移到温度为60 ℃的烘箱中,干燥2 h后得到最终产品。7. Constant temperature and humidity box-oven storage and drying of the washed gum arabic: place the washed product in a constant temperature and humidity box with a temperature of 60 °C and a humidity of 75% for 24 hours; then transfer to a temperature of 60 °C The final product was obtained after drying in an oven for 2 h.
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| CN109180837A (en) * | 2018-07-05 | 2019-01-11 | 华侨大学 | A method of adjusting Ago-Gel transparency |
| CN110028596A (en) * | 2019-04-26 | 2019-07-19 | 上海交通大学 | A kind of corn fiber gum emulsifier and preparation method thereof that structured lipid is modified |
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