CN113549496B - High-stability grease composition and preparation method thereof - Google Patents
High-stability grease composition and preparation method thereof Download PDFInfo
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- CN113549496B CN113549496B CN202110807782.XA CN202110807782A CN113549496B CN 113549496 B CN113549496 B CN 113549496B CN 202110807782 A CN202110807782 A CN 202110807782A CN 113549496 B CN113549496 B CN 113549496B
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- 239000004519 grease Substances 0.000 title claims abstract description 38
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 229920000881 Modified starch Polymers 0.000 claims abstract description 25
- 239000004368 Modified starch Substances 0.000 claims abstract description 25
- 235000019426 modified starch Nutrition 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 238000001694 spray drying Methods 0.000 claims abstract description 16
- 229930006000 Sucrose Natural products 0.000 claims abstract description 15
- 239000005720 sucrose Substances 0.000 claims abstract description 15
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 102000011632 Caseins Human genes 0.000 claims abstract description 12
- 108010076119 Caseins Proteins 0.000 claims abstract description 12
- 229940080237 sodium caseinate Drugs 0.000 claims abstract description 12
- -1 sucrose ester Chemical class 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000010008 shearing Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 239000003921 oil Substances 0.000 claims description 20
- 235000019198 oils Nutrition 0.000 claims description 20
- 239000003963 antioxidant agent Substances 0.000 claims description 15
- 230000003078 antioxidant effect Effects 0.000 claims description 15
- 235000006708 antioxidants Nutrition 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 15
- 239000000945 filler Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 14
- 229920002261 Corn starch Polymers 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- 239000008120 corn starch Substances 0.000 claims description 14
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 12
- 235000013616 tea Nutrition 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 claims description 10
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 claims description 10
- 229940114124 ferulic acid Drugs 0.000 claims description 10
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 claims description 10
- 235000001785 ferulic acid Nutrition 0.000 claims description 10
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 7
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 6
- 238000007792 addition Methods 0.000 claims description 6
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical group CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 claims description 5
- 235000019197 fats Nutrition 0.000 claims description 5
- 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 claims description 4
- 235000019864 coconut oil Nutrition 0.000 claims description 4
- 239000003240 coconut oil Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- QAQJMLQRFWZOBN-LAUBAEHRSA-N L-ascorbyl-6-palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](O)[C@H]1OC(=O)C(O)=C1O QAQJMLQRFWZOBN-LAUBAEHRSA-N 0.000 claims description 3
- 239000011786 L-ascorbyl-6-palmitate Substances 0.000 claims description 3
- 229930003427 Vitamin E Natural products 0.000 claims description 3
- 235000010385 ascorbyl palmitate Nutrition 0.000 claims description 3
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 3
- 235000013824 polyphenols Nutrition 0.000 claims description 3
- 235000019165 vitamin E Nutrition 0.000 claims description 3
- 229940046009 vitamin E Drugs 0.000 claims description 3
- 239000011709 vitamin E Substances 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 235000019498 Walnut oil Nutrition 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000008170 walnut oil Substances 0.000 claims description 2
- 244000269722 Thea sinensis Species 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 2
- 241001122767 Theaceae Species 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- 235000013336 milk Nutrition 0.000 description 9
- 239000008267 milk Substances 0.000 description 9
- 210000004080 milk Anatomy 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 235000021539 instant coffee Nutrition 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 235000016213 coffee Nutrition 0.000 description 3
- 235000013353 coffee beverage Nutrition 0.000 description 3
- 210000000795 conjunctiva Anatomy 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 235000021243 milk fat Nutrition 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 2
- 230000003859 lipid peroxidation Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000008172 hydrogenated vegetable oil Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 125000000185 sucrose group Chemical group 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 235000008939 whole milk Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0092—Mixtures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Abstract
The invention relates to a high-stability grease composition and a preparation method thereof, belonging to the technical field of food processing, wherein the composition comprises the following raw materials: modified starch, deionized water, sodium caseinate, a grease component, monoglyceride, sucrose ester and an additive; the preparation method of the composition comprises the following steps: firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase; secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 10-20min to obtain an oil phase; and thirdly, mixing the water phase and the oil phase, adding the additive into the mixture by high-speed shearing for 5min, homogenizing, and putting the homogenized emulsion into a spray drying tower for spray drying to obtain the high-stability grease composition. The high-stability grease component prepared by the invention has good shelf life stability, good embedding property and long product shelf life.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a high-stability grease composition and a preparation method thereof.
Background
In recent years, the demand of people for instant coffee and milk tea is increasing, and meanwhile, the production and marketing of vegetable fat powder (liquid or solid) which is a main raw material of the instant coffee and milk tea is also increasing, and the instant coffee and milk tea mainly occurs in tea restaurants, coffee houses and terminal retail products, namely, consumers consume the instant coffee and milk tea at the first time, so that the instant coffee and milk tea have no problem of shelf life in a liquid state. The instant coffee and milk tea are in liquid state, the packaging form is mainly PET, a tetra pack and an iron pot, the shelf life is 9-12 months, more fat floats in the shelf life, the quality of the product is seriously influenced, the product mainly comprises tea, coffee, milk or whole milk powder, the fat floats in the milk, the milk fat is controlled to have a certain effect through an emulsifying agent and colloid, but the milk fat is a very complex grease system, and meanwhile, the emulsifying state of grease is greatly changed, so that great difficulty is brought to process control.
The emulsified grease takes hydrogenated vegetable oil with higher purity as an emulsifying object, and a fat product with higher emulsion stability can be obtained through a proper emulsion formula and a high-efficiency emulsification process, but the stability of the emulsified grease in the current market can not meet the requirements of instant liquid products, the emulsified grease with high stability can completely replace milk fat, can adapt to the process requirements of instant milk tea and coffee, improves the shelf life stability of the product, and can have more choices in flavor and excellent shelf life.
Disclosure of Invention
The invention aims to provide a high-stability grease composition and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
the high-stability grease composition comprises the following raw materials in parts by weight:
50-90 parts of modified starch, 50-80 parts of deionized water, 1-10 parts of sodium caseinate, 40-80 parts of grease component, 0.5-3 parts of monoglyceride, 0.6-2 parts of sucrose ester and 10-15 parts of additive;
further, the modified starch is prepared by the steps of:
step S11, mixing sodium hydroxide, ferulic acid and deionized water, adding acetic anhydride, stirring at 20 ℃ for reaction for 1h, regulating the pH value to 2 by using concentrated hydrochloric acid with the mass fraction of 37% after the reaction is finished, standing for 30min, carrying out vacuum filtration, and washing a filter cake by using deionized water to obtain an intermediate 1; wherein the dosage ratio of sodium hydroxide, ferulic acid, deionized water and acetic anhydride is 2.5g:3.8g:20mL:2.4mL;
the reaction process is as follows:
step S12, mixing the intermediate 1, thionyl chloride and chloroform, then adding N, N-dimethylformamide, heating to 55 ℃, stirring for reaction for 8 hours, cooling to room temperature after the reaction is finished, and concentrating under reduced pressure to remove a solvent to obtain an intermediate 2; wherein, the dosage ratio of the intermediate 1, the thionyl chloride, the chloroform and the N, N-dimethylformamide is 2.9g:2mL:20mL:20mg;
the reaction process is as follows:
step S13, drying corn starch to constant weight at 60 ℃, mixing the dried corn starch with pyridine, refluxing and stirring for 1-2 hours at 110 ℃, then reducing the temperature to 0 ℃, adding intermediate 2, refluxing and stirring for 4-6 hours at 95 ℃ after the addition, washing with absolute ethyl alcohol and distilled water in sequence after the reaction is finished, then putting the product into a Soxhlet extractor, extracting for 8 hours with acetone, and then drying in vacuum for 24 hours to obtain solid a; wherein, the dosage ratio of the corn starch, the pyridine and the intermediate 2 is 5g:60mL:6-10g;
and S14, treating the solid a to obtain the modified starch.
Further, the specific steps of the processing in step S14 are as follows:
mixing the solid a with distilled water, adding sodium hydroxide to adjust the pH value to 9, heating to 30 ℃, stirring and reacting for 50-60min, then dripping an auxiliary agent, adding a sodium hydroxide solution with the mass fraction of 3% to maintain the pH value of the system to be about 8.5 in the dripping process, reacting for 4h, adjusting the pH value to 6 by using a hydrochloric acid solution with the mass fraction of 3% after the reaction is finished, washing by using distilled water and absolute ethyl alcohol in sequence until no chloride ions are detected in a washing liquid, and drying to constant weight at 45 ℃ after the washing is finished.
Further, the dosage ratio of the solid a, distilled water and auxiliary agent is 10g:20mL:31-32mL.
Further, the additive is a filler and an antioxidant, and the dosage mass ratio of the filler to the antioxidant is 100:2-3.
Further, the filler is one or two of glucose and sucrose mixed according to any proportion, and the antioxidant is one or more of vitamin E, ascorbyl palmitate and tea polyphenol mixed according to any proportion.
Further, the oil component is one of coconut oil and walnut oil.
Further, the auxiliary agent is octenyl succinic anhydride and isopropanol according to the dosage ratio of 1g:10mL of the mixture.
A preparation method of a high-stability grease composition comprises the following steps:
firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase;
secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 10-20min to obtain an oil phase;
thirdly, mixing the water phase and the oil phase, adding the additive by high-speed shearing for 5min under the condition of the rotating speed of 10000r/min, homogenizing, and putting the homogenized emulsion into a spray drying tower for spray drying to obtain the high-stability grease composition.
Further, the homogenization condition is that the temperature is 70-80 ℃ and the pressure is 15-20MPa; the air inlet temperature is 190 ℃ and the feeding temperature is 60 ℃ during spray drying.
The invention has the beneficial effects that:
in the process of preparing the grease composition, a modified starch is prepared, the modified starch takes corn starch as a matrix, ferulic acid as a raw material, acetic anhydride is used for protecting hydroxyl groups on a molecular structure of the ferulic acid, acyl chloride is introduced into the corn starch to prepare an intermediate 2, the intermediate 2 and starch undergo a grafting reaction, the ferulic acid is introduced into the starch, the oxidation resistance of the starch is improved, lipid peroxidation free radicals are eliminated, so that the lipid peroxidation process is stopped or delayed, a solid a is prepared, deacetylation protection is carried out under an alkaline condition, and simultaneously, esterification reaction is carried out between the starch and octenyl succinic anhydride under the alkaline condition, so that the modified starch is prepared. The high-stability grease composition provided by the invention provides emulsified grease with high stability, and avoids fat floating in the shelf life, so that the shelf life stability of the product is improved; in addition, the embedding property is good, the shelf life of the product is long, and the stability is good.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing modified starch:
step S11, mixing sodium hydroxide, ferulic acid and deionized water, adding acetic anhydride, stirring at 20 ℃ for reaction for 1h, regulating the pH value to 2 by using concentrated hydrochloric acid with the mass fraction of 37% after the reaction is finished, standing for 30min, carrying out vacuum filtration, and washing a filter cake by using deionized water to obtain an intermediate 1; wherein the dosage ratio of sodium hydroxide, ferulic acid, deionized water and acetic anhydride is 2.5g:3.8g:20mL:2.4mL;
step S12, mixing the intermediate 1, thionyl chloride and chloroform, then adding N, N-dimethylformamide, heating to 55 ℃, stirring for reaction for 8 hours, cooling to room temperature after the reaction is finished, and concentrating under reduced pressure to remove a solvent to obtain an intermediate 2; wherein, the dosage ratio of the intermediate 1, the thionyl chloride, the chloroform and the N, N-dimethylformamide is 2.9g:2mL:20mL:20mg;
step S13, drying corn starch to constant weight at 60 ℃, mixing the dried corn starch with pyridine, refluxing and stirring for 1h at 110 ℃, then reducing the temperature to 0 ℃, adding an intermediate 2, refluxing and stirring for 4h at 95 ℃ after the addition, washing with absolute ethyl alcohol and distilled water in sequence after the reaction is finished, then placing the product into a Soxhlet extractor, extracting for 8h with acetone, and then drying in vacuum for 24h to obtain a solid a; wherein, the dosage ratio of the corn starch, the pyridine and the intermediate 2 is 5g:60mL:6g;
and S14, mixing the solid a with distilled water, adding sodium hydroxide to adjust the pH value to 9, heating to 30 ℃, stirring and reacting for 50min, then dripping an auxiliary agent, adding a sodium hydroxide solution with the mass fraction of 3% in the dripping process to maintain the pH value of the system to be about 8.5, reacting for 4h, adjusting the pH value to 6 by using a hydrochloric acid solution with the mass fraction of 3% after the reaction is finished, washing by using distilled water and absolute ethyl alcohol in sequence, and drying to constant weight at the temperature of 45 ℃ after the washing is finished. Wherein the dosage ratio of the solid a to the distilled water to the auxiliary agent is 10g:20mL:31mL. The auxiliary agent is octenyl succinic anhydride and isopropanol according to the dosage ratio of 1g:10mL of the mixture.
Example 2
Preparing modified starch:
step S11, mixing sodium hydroxide, ferulic acid and deionized water, adding acetic anhydride, stirring at 20 ℃ for reaction for 1h, regulating the pH value to 2 by using concentrated hydrochloric acid with the mass fraction of 37% after the reaction is finished, standing for 30min, carrying out vacuum filtration, and washing a filter cake by using deionized water to obtain an intermediate 1; wherein the dosage ratio of sodium hydroxide, ferulic acid, deionized water and acetic anhydride is 2.5g:3.8g:20mL:2.4mL;
step S12, mixing the intermediate 1, thionyl chloride and chloroform, then adding N, N-dimethylformamide, heating to 55 ℃, stirring for reaction for 8 hours, cooling to room temperature after the reaction is finished, and concentrating under reduced pressure to remove a solvent to obtain an intermediate 2; wherein, the dosage ratio of the intermediate 1, the thionyl chloride, the chloroform and the N, N-dimethylformamide is 2.9g:2mL:20mL:20mg;
step S13, drying corn starch to constant weight at 60 ℃, mixing the dried corn starch with pyridine, refluxing and stirring for 2 hours at 110 ℃, then reducing the temperature to 0 ℃, adding an intermediate 2, refluxing and stirring for 6 hours at 95 ℃ after the addition, washing with absolute ethyl alcohol and distilled water in sequence after the reaction is finished, then placing the product into a Soxhlet extractor, extracting for 8 hours with acetone, and then drying in vacuum for 24 hours to obtain a solid a; wherein, the dosage ratio of the corn starch, the pyridine and the intermediate 2 is 5g:60mL:10g;
and S14, mixing the solid a with distilled water, adding sodium hydroxide to adjust the pH value to 9, heating to 30 ℃, stirring and reacting for 60min, then dripping an auxiliary agent, adding a sodium hydroxide solution with the mass fraction of 3% in the dripping process to maintain the pH value of the system to be about 8.5, reacting for 4h, adjusting the pH value to 6 by using a hydrochloric acid solution with the mass fraction of 3% after the reaction is finished, washing by using distilled water and absolute ethyl alcohol in sequence, and drying to constant weight at the temperature of 45 ℃ after the washing is finished. Wherein the dosage ratio of the solid a to the distilled water to the auxiliary agent is 10g:20mL:32mL. The auxiliary agent is octenyl succinic anhydride and isopropanol according to the dosage ratio of 1g:10mL of the mixture.
Example 3
Preparing a high-stability grease composition:
firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase;
secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 10min to obtain an oil phase;
thirdly, mixing the water phase and the oil phase, adding the additive in the condition of high-speed shearing for 5min under the condition of the rotating speed of 10000r/min, and homogenizing at the temperature of 70 ℃ and the pressure of 15MPa; and (3) feeding the homogenized emulsion into a spray drying tower for spray drying, wherein the air inlet temperature is 190 ℃ and the feeding temperature is 60 ℃ during spray drying, so as to obtain the high-stability grease composition.
Wherein the weight parts of each substance are 50 parts of modified starch, 50 parts of deionized water, 1 part of sodium caseinate, 40 parts of grease component, 0.5 part of monoglyceride, 0.6 part of sucrose ester and 10 parts of additive;
wherein the modified starch is prepared in example 2; the additive is filler and antioxidant, and the dosage mass ratio of the filler to the antioxidant is 100:2; the filler is glucose, and the antioxidant is vitamin E; the oil component is coconut oil.
Example 4
Preparing a high-stability grease composition:
firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase;
secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 15min to obtain an oil phase;
thirdly, mixing the water phase and the oil phase, adding the additive in the condition of high-speed shearing for 5min under the condition of the rotating speed of 10000r/min, and homogenizing at the temperature of 75 ℃ and the pressure of 18MPa; and (3) feeding the homogenized emulsion into a spray drying tower for spray drying, wherein the air inlet temperature is 190 ℃ and the feeding temperature is 60 ℃ during spray drying, so as to obtain the high-stability grease composition.
Wherein the weight parts of each substance are 70 parts of modified starch, 80 parts of deionized water, 5 parts of sodium caseinate, 60 parts of grease component, 2 parts of monoglyceride, 1 part of sucrose ester and 12 parts of additive;
wherein the modified starch is prepared in example 2; the additive is filler and antioxidant, and the dosage mass ratio of the filler to the antioxidant is 100:2.5; the filler is glucose, and the antioxidant is ascorbyl palmitate; the oil component is coconut oil.
Example 5
Preparing a high-stability grease composition:
firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase;
secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 20min to obtain an oil phase;
thirdly, mixing the water phase and the oil phase, adding the additive in the condition of high-speed shearing for 5min under the condition of the rotating speed of 10000r/min, and homogenizing at the temperature of 80 ℃ and the pressure of 20MPa; and (3) feeding the homogenized emulsion into a spray drying tower for spray drying, wherein the air inlet temperature is 190 ℃ and the feeding temperature is 60 ℃ during spray drying, so as to obtain the high-stability grease composition.
Wherein the weight parts of each substance are 90 parts of modified starch, 80 parts of deionized water, 10 parts of sodium caseinate, 80 parts of grease component, 3 parts of monoglyceride, 2 parts of sucrose ester and 15 parts of additive;
wherein the modified starch is prepared in example 2; the additive is filler and antioxidant, and the dosage mass ratio of the filler to the antioxidant is 100:3, a step of; the filler is sucrose, and the antioxidant is tea polyphenol; the oil component is oleum Juglandis.
Comparative example 1
The modified starch of example 4 was replaced with starch octenyl succinate, the remaining raw materials and the preparation process were kept unchanged.
Comparative example 2
The modified starch of example 4 was replaced with corn starch, the remaining materials and preparation process remained unchanged.
The samples prepared in examples 3 to 5 and comparative examples 1 to 2 were tested, 40g of the sample was mixed with 200mL of hot water at 80℃and then 20% by mass of citric acid was added dropwise, and the emulsion was observed after adjusting the pH to 3;
the results are shown in table 1 below:
TABLE 1
| Emulsion character | |
| Example 3 | Even and fine liquid, no conjunctiva layering and no particle wall hanging |
| Example 4 | Even and fine liquid, no conjunctiva layering and no particle wall hanging |
| Example 5 | Even and fine liquid, no conjunctiva layering and no particle wall hanging |
| Comparative example 1 | Even and fine liquid, slightly layered, no particle wall hanging |
| Comparative example 2 | Serious layering phenomenon, serious particle wall hanging and oil precipitation phenomenon on the surface |
The acid value and the peroxide value of the samples obtained in example 4 and comparative example 1 were measured, and the acid value and the peroxide value were measured with reference to GB5009.229-2016 and GB5009.227-2016, respectively, and the test results are shown in Table 2 below:
the test results are shown in table 2 below:
TABLE 2
| Example 4 | Comparative example 1 | |
| Acid value (KOH)/(mg/g) | 0.35 | 0.78 |
| Peroxide value/(mmol/kg) | 0.19 | 0.97 |
The high-stability grease composition is better in acid resistance and more stable.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (6)
1. The high-stability grease composition comprises the following raw materials in parts by weight: 50-90 parts of modified starch, 50-80 parts of deionized water, 1-10 parts of sodium caseinate, 40-80 parts of grease component, 0.5-3 parts of monoglyceride, 0.6-2 parts of sucrose ester and 10-15 parts of additive; the modified starch is characterized by being prepared by the following steps:
step S11, mixing sodium hydroxide, ferulic acid and deionized water, adding acetic anhydride, and stirring at 20 ℃ for reaction for 1h after the addition to obtain an intermediate 1;
step S12, mixing the intermediate 1, thionyl chloride and chloroform, then adding N, N-dimethylformamide, heating to 55 ℃, and stirring for reaction for 8 hours to obtain an intermediate 2;
step S13, drying corn starch to constant weight at 60 ℃, mixing the dried corn starch with pyridine, refluxing and stirring for 1-2h at 110 ℃, then reducing the temperature to 0 ℃, adding intermediate 2, and refluxing and stirring for 4-6h at 95 ℃ after the addition to obtain solid a;
s14, mixing the solid a with distilled water, adding sodium hydroxide to adjust the pH value to 9, heating to 30 ℃, stirring and reacting for 50-60min, then dripping an auxiliary agent, reacting for 4h, adjusting the pH value to 6 by using a hydrochloric acid solution with the mass fraction of 3% after the reaction is finished, washing by using distilled water and absolute ethyl alcohol in sequence, and drying to constant weight at 45 ℃ after the washing is finished; the dosage ratio of the solid a, distilled water and the auxiliary agent is 10g:20mL:31-32mL; the auxiliary agent is octenyl succinic anhydride and isopropanol according to the dosage ratio of 1g:10mL of the mixture.
2. The high-stability grease composition according to claim 1, wherein the additive is a filler and an antioxidant, and the mass ratio of the filler to the antioxidant is 100:2-3.
3. The high-stability grease composition according to claim 2, wherein the filler is one or both of glucose and sucrose, and the antioxidant is one or more of vitamin E, ascorbyl palmitate and tea polyphenol.
4. The high stability grease composition according to claim 1, wherein the grease component is one of coconut oil and walnut oil.
5. The method for preparing a high-stability grease composition according to claim 1, comprising the steps of:
firstly, mixing modified starch and deionized water, heating to 60 ℃, then adding sodium caseinate, and stirring for 3min to obtain a water phase;
secondly, heating the oil component to 70 ℃, then adding monoglyceride and sucrose ester, and stirring for 10-20min to obtain an oil phase;
thirdly, mixing the water phase and the oil phase, adding the additive by high-speed shearing for 5min under the condition of the rotating speed of 10000r/min, homogenizing, and carrying out spray drying on the homogenized emulsion to obtain the high-stability grease composition.
6. The method for producing a high-stability fat composition according to claim 5, wherein the homogenization is carried out at a temperature of 70 to 80℃and a pressure of 15 to 20MPa; the air inlet temperature is 190 ℃ and the feeding temperature is 60 ℃ during spray drying.
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| CN104277127A (en) * | 2013-07-10 | 2015-01-14 | 江苏宝宝宿迁国民生物科技有限公司 | Preparation method for oxidized esterified rice starch |
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| CN104054849A (en) * | 2014-05-21 | 2014-09-24 | 上海英莱腾医药研究有限公司 | High-content medium chain triglyceride powdered oil and preparation method thereof |
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