CN116098269A - Instant freeze-dried fish gelatin and preparation method thereof - Google Patents
Instant freeze-dried fish gelatin and preparation method thereof Download PDFInfo
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- CN116098269A CN116098269A CN202310168879.XA CN202310168879A CN116098269A CN 116098269 A CN116098269 A CN 116098269A CN 202310168879 A CN202310168879 A CN 202310168879A CN 116098269 A CN116098269 A CN 116098269A
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- fish gelatin
- treatment
- foaming
- parts
- drying
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- 241000251468 Actinopterygii Species 0.000 title claims abstract description 100
- 108010010803 Gelatin Proteins 0.000 title claims abstract description 98
- 229920000159 gelatin Polymers 0.000 title claims abstract description 98
- 239000008273 gelatin Substances 0.000 title claims abstract description 98
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 98
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000011282 treatment Methods 0.000 claims abstract description 70
- 238000005187 foaming Methods 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000001035 drying Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- 238000007710 freezing Methods 0.000 claims abstract description 24
- 230000008014 freezing Effects 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims description 57
- 239000000047 product Substances 0.000 claims description 55
- 239000002131 composite material Substances 0.000 claims description 44
- 238000005266 casting Methods 0.000 claims description 40
- 238000006116 polymerization reaction Methods 0.000 claims description 38
- 239000000440 bentonite Substances 0.000 claims description 35
- 229910000278 bentonite Inorganic materials 0.000 claims description 35
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 238000005859 coupling reaction Methods 0.000 claims description 30
- 239000004800 polyvinyl chloride Substances 0.000 claims description 30
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 30
- 239000002244 precipitate Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000004833 fish glue Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 claims description 18
- 238000007112 amidation reaction Methods 0.000 claims description 18
- -1 hydroxyl bentonite Chemical compound 0.000 claims description 18
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- FQGPWDVZYOJHCB-UHFFFAOYSA-N 3-methylbut-3-enamide Chemical compound CC(=C)CC(N)=O FQGPWDVZYOJHCB-UHFFFAOYSA-N 0.000 claims description 12
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 230000008878 coupling Effects 0.000 claims description 12
- 238000010168 coupling process Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- KIJDMKUPUUYDLN-UHFFFAOYSA-N 2,2-dimethyl-4-trimethoxysilylbutan-1-amine Chemical compound CO[Si](OC)(OC)CCC(C)(C)CN KIJDMKUPUUYDLN-UHFFFAOYSA-N 0.000 claims description 10
- CSFUYRGXBNPTSR-UHFFFAOYSA-N 2-bromohexanoyl bromide Chemical compound CCCCC(Br)C(Br)=O CSFUYRGXBNPTSR-UHFFFAOYSA-N 0.000 claims description 10
- 238000004332 deodorization Methods 0.000 claims description 10
- 239000003480 eluent Substances 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 238000009461 vacuum packaging Methods 0.000 claims description 7
- 230000009435 amidation Effects 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 4
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 4
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 150000001262 acyl bromides Chemical group 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 125000001246 bromo group Chemical class Br* 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 4
- 235000015097 nutrients Nutrition 0.000 abstract description 4
- 230000009182 swimming Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000001953 sensory effect Effects 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 102000008186 Collagen Human genes 0.000 description 3
- 108010035532 Collagen Proteins 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229920001436 collagen Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005956 quaternization reaction Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012549 training Methods 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000251730 Chondrichthyes Species 0.000 description 1
- 244000000626 Daucus carota Species 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 229920002683 Glycosaminoglycan Polymers 0.000 description 1
- 206010059013 Nocturnal emission Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010976 amide bond formation reaction Methods 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 235000005770 birds nest Nutrition 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 235000004213 low-fat Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000005765 wild carrot Nutrition 0.000 description 1
Classifications
-
- 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
- A23L17/00—Food-from-the-sea products; Fish products; Fish meal; Fish-egg substitutes; Preparation or treatment thereof
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
- A23L5/273—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/55—Rehydration or dissolving of foodstuffs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Zoology (AREA)
- Marine Sciences & Fisheries (AREA)
- Mycology (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Freezing, Cooling And Drying Of Foods (AREA)
Abstract
The invention discloses instant freeze-dried fish gelatin and a preparation method thereof, and belongs to the technical field of aquatic food products. The preparation method comprises the steps of rehydration, foaming treatment, fishy smell removal treatment, freeze-drying and drying of the fish gelatin. The invention adopts the ultralow temperature liquid nitrogen freezing process, shortens the freeze-drying time, and the prepared freeze-dried fish gelatin has beautiful color, greatly retains the nutrient components, has high rehydration rate and is convenient and fast to use.
Description
Technical Field
The invention relates to the technical field of aquatic food products, in particular to instant freeze-dried fish gelatin and a preparation method thereof.
Background
The fish glue is also called as flower glue and is a dried product of swimming bladder. The main components of the fish gelatin are high-grade collagen and mucopolysaccharide substances, various vitamins and various microelements such as calcium, zinc, iron, selenium and the like, and the fish gelatin is considered to be sweet in taste by the traditional Chinese medicine, has the effects of nourishing blood, stopping bleeding, tonifying kidney and stopping nocturnal emission, and is suitable for pregnant women, old people and people with deficiency of both qi and blood and anemia.
Chinese patent CN107568638A discloses a method for preparing freeze-dried fish gelatin, which mainly comprises the following steps: the preparation method comprises the steps of steaming, foaming, quick freezing, freeze drying and packaging finished products, the pretreatment effect is good, the fish gelatin can be foamed for 4-5 times, meanwhile, the problem of bacterial infection is solved in the foaming process, the obtained fish gelatin forms a porous dry material state, the hydrophilicity is high, the fish gelatin is convenient and easy to cook during cooking, meanwhile, the collagen and various nutrient elements of the fish gelatin are reserved, and the fish gelatin can be used for edge beating or boiling.
Chinese patent CN104432223a provides an instant flavor swimming bladder tablet and its preparation method, comprising the following steps: (1) cleaning and removing impurities; (2) rinsing to remove fishy smell; (3) drying; (4) a filler; (5) tabletting; (6) slurry hanging; (7) quick freezing; (8) vacuum frying and deoiling; and (9) cooling, packaging and the like. The invention adopts the modes of filling the seasonings in the swimming bladder, tabletting, shaping and pulping the swimming bladder, can endow the swimming bladder with different flavors, and simultaneously can maintain the swimming bladder in a uniform sheet shape after frying and puffing, so that the swimming bladder not only maintains the original nutritional value, but also has better sensory quality.
The prior art adopts a common freeze-drying process, the treatment time is longer, and meanwhile, the fishy smell in the fish gelatin is difficult to remove by common rinsing, so that the edible experience of the finished product is seriously influenced.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides an instant freeze-dried fish gelatin and a preparation method thereof.
A preparation method of instant freeze-dried fish gelatin comprises the following steps:
1) The fish gelatin is placed in a saturated steam environment for 10-30 min for rehydration, the rehydrated fish gelatin is transferred into a foaming pool containing 75-90 ℃ water for foaming treatment, a composite adsorption film is adopted for deodorization treatment in the foaming treatment process, and the foaming treatment is finished and filtered and recovered to obtain the foaming fish gelatin for later use;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow-temperature liquid nitrogen freezing treatment, so that the frozen fish glue is obtained; and drying the frozen fish gelatin to obtain the freeze-dried fish gelatin, and vacuum packaging to obtain the instant freeze-dried fish gelatin.
Preferably, in the foaming treatment in step 1), the mass ratio of the fish gelatin to water after rehydration is 1: (45-70) g/g, and the treatment time is 4-10 h.
Preferably, in the deodorization treatment in the step 1), the ratio of the film width of the composite adsorption film to the bottom area of the foaming tank is 0.2-0.5 m:1m 2 The height of the composite adsorption film is equal to the water depth of the foaming pool.
Preferably, the temperature of the ultralow-temperature liquid nitrogen freezing treatment in the step 2) is between-210 ℃ and-196 ℃, and the treatment time is between 10 and 30 minutes.
Preferably, in the step 2), the drying is carried out at 35-45 ℃ for 25-35 hours;
the invention adopts the ultralow temperature liquid nitrogen freezing process, greatly shortens the freeze-drying time, and the prepared freeze-dried fish gelatin has beautiful color, greatly reserves the nutrient components, has high rehydration rate and is convenient and fast to use.
In the preparation process of the composite adsorption film, firstly, alkaline liquor is used for treating bentonite to introduce hydroxyl and obtain hydroxyl bentonite, then the hydroxyl bentonite and 4-amino-3, 3-dimethylbutyl trimethoxy silane are subjected to coupling reaction, the coupled product is subsequently reacted with 2-bromohexanoyl bromide, amide bonds are formed by substituting bromine atoms of acyl bromide groups for connection, and the obtained amidated product is polymerized with 3-methyl-3-butenamide and triethylene glycol diacrylate under catalysis to obtain a polymerization product; finally, the polymerization product, polyvinyl chloride and solvent are mixed to prepare casting solution, and the composite adsorption film is prepared by a solution casting method.
The fishy smell source in the fish glue is mainly substances such as organic amine, trimethylamine and the like generated by protein decomposition, the removal of the fishy smell substances by the traditional adsorption materials such as porous carbon is dominant by physical adsorption, the physical adsorption is greatly influenced by temperature, and the adsorption of the common physical adsorption materials to the organic amine is poor at the foaming temperature of the process. The invention adopts polyvinyl chloride, and enhances the fixation of the adsorption film to organic amine by quaternization based on the reactivity of carbon-chlorine bonds. The hydrophilicity of the polyvinyl chloride film is insufficient, so that the bentonite-based polymer material is used for assisting the polyvinyl chloride film to form a porous structure, and the hydrophilicity, roughness and porosity of the film are further improved; the hydroxyl bentonite reacts with 4-amino-3, 3-dimethylbutyl trimethoxy silane and 2-bromohexanoyl bromide, and then is polymerized with 3-methyl-3-butenamide and triethylene glycol diacrylate, and the alkyl branched structure and ether oxygen bond are beneficial to improving the dispersibility among particles of a polymerization product, preventing the agglomeration of bentonite and forming a loose microstructure. The composite adsorption film prepared by the solution casting method has good hydrophilicity and microscopic pores, can improve the surface roughness of the film, is more effectively combined with water in a foaming pool and adsorbs fishy smell substances, and achieves the aim of removing fishy smell.
Preferably, the preparation method of the composite adsorption film comprises the following steps of:
s1, uniformly mixing bentonite and a sodium hydroxide aqueous solution, heating for heat treatment, centrifuging, collecting precipitate, washing the precipitate until eluent is neutral, and drying to obtain hydroxyl bentonite for later use;
s2, taking the hydroxyl bentonite and toluene to be uniformly mixed, adding 4-amino-3, 3-dimethylbutyl trimethoxy silane under the anaerobic condition, and then carrying out coupling reaction under the reflux condition; after the coupling reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain a coupling product for later use;
s3, mixing the coupling product, the acid binding agent and toluene uniformly, and adding 2-bromohexanoyl bromide for amidation reaction; after the amidation reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate with acetone, and drying to obtain an amidation product for later use;
s4, under the anaerobic condition, the amidation product, the catalyst and N, N-dimethylformamide are additionally taken and uniformly mixed, and then 3-methyl-3-butenamide is added for polymerization reaction; filtering and collecting a filter cake after the polymerization reaction is finished, washing and drying the filter cake by acetone to obtain a polymerization product for later use;
s5, mixing the polymerization product, polyvinyl chloride and N, N-dimethylacetamide in proportion, uniformly dispersing the components after heating and melting, and degassing to obtain a casting solution; casting the casting solution on a substrate, uniformly coating by coating equipment, drying and rolling to obtain the composite adsorption film.
Further, the preparation method of the composite adsorption film comprises the following steps of:
s1, uniformly mixing 2.55-3.60 parts of bentonite with 45-60 parts of sodium hydroxide aqueous solution, heating, performing heat treatment, centrifuging, collecting precipitate, washing the precipitate until eluent is neutral, and drying to obtain hydroxyl bentonite for later use;
s2, taking 2.75-3.70 parts of the hydroxyl bentonite and 100-150 parts of toluene, uniformly mixing, adding 2.20-2.95 parts of 4-amino-3, 3-dimethylbutyl trimethoxy silane under the protection of nitrogen, and then carrying out coupling reaction under the condition of reflux; after the coupling reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain a coupling product for later use;
s3, taking 2.15-2.80 parts of the coupling product, 3.15-4.05 parts of triethylamine and 60-90 parts of toluene, uniformly mixing, adding 3.85-5.00 parts of 2-bromohexanoyl bromide, and carrying out amidation reaction; after the amidation reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate with acetone at 0-4 ℃, and drying to obtain an amidation product for later use;
under the protection of S4 and nitrogen, 2.45 to 3.45 parts of amidated products, 1.70 to 2.40 parts of 2,2' -bipyridine, 0.75 to 1.05 parts of cuprous bromide and 125 to 175 parts of N, N-dimethylformamide are taken, evenly mixed, and after the color of the mixed solution turns into dark brown, 4.40 to 6.15 parts of 3-methyl-3-butenamide and 0.65 to 0.90 part of triethylene glycol diacrylate are added for polymerization reaction; filtering and collecting a filter cake after the polymerization reaction is finished, washing the filter cake by acetone at 0-4 ℃ and drying to obtain a polymerization product for later use;
s5, mixing the polymerization product, polyvinyl chloride and N, N-dimethylacetamide in proportion, uniformly dispersing the components after heating and melting, and degassing to obtain a casting solution; casting the casting solution on a substrate, uniformly coating by coating equipment, drying and rolling to obtain the composite adsorption film.
Preferably, the concentration of the aqueous sodium hydroxide solution in the step S1 is 0.5-1.0 mol/L.
Preferably, the temperature of the heat treatment in the step S1 is 40-65 ℃ and the treatment time is 0.5-2 h.
Preferably, the temperature of the coupling reaction in the step S2 is 110-125 ℃, and the reaction time is 12-24 hours.
Preferably, the amidation reaction temperature in the step S3 is 0-15 deg.C and the reaction time is 6-18 h.
Preferably, the polymerization reaction temperature in the step S4 is 55-70 ℃ and the reaction time is 3-8 h.
The casting solution in the step S5 comprises the following components in percentage by mass: 0.15 to 1.80 weight percent of polymerization product, 10.5 to 15.0 weight percent of polyvinyl chloride and the balance of N, N-dimethylacetamide; preferably 0.85wt% of the polymerization product, 12.25wt% of polyvinyl chloride, and the balance N, N-dimethylacetamide.
Preferably, the polyvinyl chloride in step S5 is of film grade.
Preferably, the thickness of the composite adsorption film in the step S5 is 50-200 μm.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the invention.
The invention has the following description and functions of partial raw materials in the formula:
fish gelatin: the dried product of the swimming bladder is rich in colloid, so the fish gelatin is also called fish maw and fish gelatin. The fish gelatin is named as eight delicacies together with bird's nest and shark's fin. The fish gelatin contains high-grade collagen, multiple vitamins, and multiple microelements such as calcium, zinc, ferrum, selenium, etc. The protein content is up to 84.2%, and the fat is only 0.2%, so that the food is ideal high-protein low-fat food. Is a raw material for supplementing and synthesizing protein for human body, and is easy to be absorbed and utilized.
The invention has the beneficial effects that:
compared with the prior art, the invention adopts the ultralow temperature liquid nitrogen freezing process, greatly shortens the freeze-drying time, and the prepared freeze-dried fish gelatin has beautiful color, greatly retains the nutrient components, has high rehydration rate and is convenient and quick to use.
Compared with the prior art, the invention adopts polyvinyl chloride, enhances the fixation of the adsorption film to the organic amine by quaternization based on the reactivity of carbon-chlorine bonds, and adopts the polymer prepared by bentonite to assist the polyvinyl chloride to form a porous structure, thereby increasing the hydrophilicity, roughness and porosity of the film.
Compared with the prior art, the invention provides a preparation method of a composite adsorption film, which comprises the steps of treating bentonite with alkali liquor to introduce hydroxyl and obtain hydroxyl bentonite, then carrying out a coupling reaction on the hydroxyl bentonite and 4-amino-3, 3-dimethylbutyl trimethoxy silane, carrying out a subsequent reaction on the coupling product and 2-bromohexanoyl bromide, and carrying out an amide bond formation by substituting a bromine atom of an acyl bromide group to connect, wherein the obtained amidated product is polymerized with 3-methyl-3-butenamide and triethylene glycol diacrylate under catalysis to obtain a polymerization product; finally, the polymerization product, polyvinyl chloride and solvent are mixed to prepare casting solution, and the composite adsorption film is prepared by a solution casting method.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The comparative example and the examples of the present invention have the following parameters of part of raw materials:
fish gelatin, cargo number: hhjhhj250, shenzhen maritime, sea-going, inc; bentonite, mesh number: 1250 mesh; polyvinyl chloride, film grade;
3-methyl-3-butenamide, CAS no: 18938-03-9, shenzhen Aituo chemical Co., ltd; sodium hydroxide aqueous solution, concentration: 0.5mol/L.
Example 1
An instant freeze-dried fish gelatin is prepared by the following method:
1) Treating fish gelatin in saturated steam for 20min to rewater, and rehydratingTransferring the fish gelatin into a foaming pool containing 80 ℃ water for foaming treatment, wherein the mass ratio of the re-hydrated fish gelatin to the water is 1:60g/g, the treatment time is 8h; in the foaming treatment process, the composite adsorption film is adopted for deodorization treatment, and the ratio of the film width of the composite adsorption film to the bottom area of the foaming pool is 0.4m:1m 2 The height of the composite adsorption film is equal to the water depth of the foaming pool; filtering and recycling after the foaming treatment is finished to obtain the foaming fish glue for standby;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow temperature liquid nitrogen freezing treatment, wherein the treatment temperature is-196 ℃, and the treatment time is 20 minutes, so that the frozen fish glue is obtained; and (5) drying the frozen fish gelatin for 30 hours at 40 ℃ to obtain the frozen fish gelatin, and vacuum packaging to obtain the instant frozen fish gelatin.
The preparation method of the composite adsorption film comprises the following steps:
s1, uniformly mixing 2.55kg of bentonite with 45kg of sodium hydroxide aqueous solution, heating to perform heat treatment, wherein the heat treatment temperature is 55 ℃, and the treatment time is 1.5h; collecting precipitate by centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain hydroxyl bentonite for later use;
s2, mixing 2.75kg of the hydroxyl bentonite with 100kg of toluene uniformly, adding 2.20kg of 4-amino-3, 3-dimethylbutyl trimethoxy silane under the protection of nitrogen, and then carrying out coupling reaction under the reflux condition, wherein the coupling reaction temperature is 115 ℃, and the reaction time is 18 hours; after the coupling reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain a coupling product for later use;
s3, mixing 2.15kg of the coupling product, 3.15kg of triethylamine and 60kg of toluene uniformly, adding 3.85kg of 2-bromohexanoyl bromide, and carrying out amidation reaction at the temperature of 5 ℃ for 12 hours; after the amidation reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate with acetone at 0 ℃, and drying to obtain an amidation product for later use;
s4, under the protection of nitrogen, 2.45kg of amidated product, 1.70kg of 2,2' -bipyridine, 0.75kg of cuprous bromide and 125kg of N, N-dimethylformamide are taken and mixed uniformly, and after the color of the mixed solution turns into dark brown, 4.40kg of 3-methyl-3-butenamide and 0.65kg of triethylene glycol diacrylate are added for polymerization reaction, wherein the polymerization reaction temperature is 65 ℃ and the reaction time is 5 hours; filtering and collecting a filter cake after the polymerization reaction is finished, washing the filter cake by using acetone at the temperature of 0 ℃, and drying to obtain a polymerization product for later use;
s5, mixing 0.85 weight percent of the polymerization product, 12.25 weight percent of polyvinyl chloride and the balance of N, N-dimethylacetamide, uniformly dispersing each component after heating and melting, and degassing to obtain a casting film liquid; casting the casting film liquid on a substrate, uniformly coating the casting film liquid by coating equipment, drying and rolling to obtain the composite adsorption film, wherein the thickness of the composite adsorption film is 100 mu m.
Example 2
An instant freeze-dried fish gelatin is prepared by the following method:
1) The fish gelatin is placed in a saturated steam environment for 20min to be rehydrated, the rehydrated fish gelatin is transferred into a foaming pool containing 80 ℃ water for foaming treatment, and the mass ratio of the rehydrated fish gelatin to the water is 1:60g/g, the treatment time is 8h; in the foaming treatment process, the composite adsorption film is adopted for deodorization treatment, and the ratio of the film width of the composite adsorption film to the bottom area of the foaming pool is 0.4m:1m 2 The height of the composite adsorption film is equal to the water depth of the foaming pool; filtering and recycling after the foaming treatment is finished to obtain the foaming fish glue for standby;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow temperature liquid nitrogen freezing treatment, wherein the treatment temperature is-196 ℃, and the treatment time is 20 minutes, so that the frozen fish glue is obtained; and (5) drying the frozen fish gelatin for 30 hours at 40 ℃ to obtain the frozen fish gelatin, and vacuum packaging to obtain the instant frozen fish gelatin.
The preparation method of the composite adsorption film comprises the following steps:
s1, uniformly mixing 3.60kg of bentonite with 60kg of sodium hydroxide aqueous solution, heating to perform heat treatment, wherein the heat treatment temperature is 55 ℃, and the treatment time is 1.5h; collecting precipitate by centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain hydroxyl bentonite for later use;
s2, mixing 3.70kg of the hydroxyl bentonite with 150kg of toluene uniformly, adding 2.95kg of 4-amino-3, 3-dimethylbutyl trimethoxy silane under the protection of nitrogen, and then carrying out coupling reaction under the reflux condition, wherein the coupling reaction temperature is 115 ℃, and the reaction time is 18 hours; after the coupling reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain a coupling product for later use;
s3, mixing 2.80kg of the coupling product, 4.05kg of triethylamine and 90kg of toluene uniformly, adding 5.00kg of 2-bromohexanoyl bromide, and carrying out amidation reaction at the temperature of 5 ℃ for 12 hours; after the amidation reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate with acetone at 0 ℃, and drying to obtain an amidation product for later use;
under the protection of nitrogen, 3.45kg of amidated product, 2.40kg of 2,2' -bipyridine, 1.05kg of cuprous bromide and 175kg of N, N-dimethylformamide are taken and mixed uniformly, and after the color of the mixed solution turns into dark brown, 6.15kg of 3-methyl-3-butenamide and 0.90kg of triethylene glycol diacrylate are added for polymerization reaction, wherein the polymerization reaction temperature is 65 ℃ and the reaction time is 5 hours; filtering and collecting a filter cake after the polymerization reaction is finished, washing the filter cake by using acetone at the temperature of 0 ℃, and drying to obtain a polymerization product for later use;
s5, mixing 0.85 weight percent of the polymerization product, 12.25 weight percent of polyvinyl chloride and the balance of N, N-dimethylacetamide, uniformly dispersing each component after heating and melting, and degassing to obtain a casting film liquid; casting the casting film liquid on a substrate, uniformly coating the casting film liquid by coating equipment, drying and rolling to obtain the composite adsorption film, wherein the thickness of the composite adsorption film is 100 mu m.
Example 3
This example is basically identical to example 1, except that the casting solution in step S5 is different in the mass percentages of the components. In this embodiment, the casting solution comprises the following components in percentage by mass: 0.15wt% of polymerization product, 10.5wt% of polyvinyl chloride and the balance of N, N-dimethylacetamide.
Example 4
This example is basically identical to example 1, except that the casting solution in step S5 is different in the mass percentages of the components. In this embodiment, the casting solution comprises the following components in percentage by mass: 1.80wt% of a polymerization product, 15.0wt% of polyvinyl chloride and the balance of N, N-dimethylacetamide.
Example 5
An instant freeze-dried fish gelatin is prepared by the following method:
1) The fish gelatin is placed in a saturated steam environment for 20min to be rehydrated, the rehydrated fish gelatin is transferred into a foaming pool containing 80 ℃ water for foaming treatment, and the mass ratio of the rehydrated fish gelatin to the water is 1:60g/g, the treatment time is 8h; in the foaming treatment process, the composite adsorption film is adopted for deodorization treatment, and the ratio of the film width of the composite adsorption film to the bottom area of the foaming pool is 0.4m:1m 2 The height of the composite adsorption film is equal to the water depth of the foaming pool; filtering and recycling after the foaming treatment is finished to obtain the foaming fish glue for standby;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow temperature liquid nitrogen freezing treatment, wherein the treatment temperature is-196 ℃, and the treatment time is 20 minutes, so that the frozen fish glue is obtained; and (5) drying the frozen fish gelatin for 30 hours at 40 ℃ to obtain the frozen fish gelatin, and vacuum packaging to obtain the instant frozen fish gelatin.
The preparation method of the composite adsorption film comprises the following steps:
mixing bentonite 0.85wt% and polyvinyl chloride 12.25wt% with the balance of N, N-dimethylacetamide, heating and melting to uniformly disperse the components, and degassing to obtain a casting solution; casting the casting film liquid on a substrate, uniformly coating the casting film liquid by coating equipment, drying and rolling to obtain the composite adsorption film, wherein the thickness of the composite adsorption film is 100 mu m.
Example 6
An instant freeze-dried fish gelatin is prepared by the following method:
1) The fish gelatin is placed in a saturated steam environment for 20min to be rehydrated, the rehydrated fish gelatin is transferred into a foaming pool containing 80 ℃ water for foaming treatment, and the mass ratio of the rehydrated fish gelatin to the water is 1:60g/g, the treatment time is 8h; in the foaming treatment process, the adsorption film is adopted for deodorization treatment, and the ratio of the film width of the adsorption film to the bottom area of the foaming pool is 0.4m:1m 2 Adsorption film height and foaming pool waterDeeply leveling; filtering and recycling after the foaming treatment is finished to obtain the foaming fish glue for standby;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow temperature liquid nitrogen freezing treatment, wherein the treatment temperature is-196 ℃, and the treatment time is 20 minutes, so that the frozen fish glue is obtained; and (5) drying the frozen fish gelatin for 30 hours at 40 ℃ to obtain the frozen fish gelatin, and vacuum packaging to obtain the instant frozen fish gelatin.
The preparation method of the adsorption film comprises the following steps:
mixing 12.25wt% of polyvinyl chloride with the balance of N, N-dimethylacetamide, heating and melting to uniformly disperse the components, and degassing to obtain a casting solution; casting the casting film liquid on a substrate, uniformly coating the casting film liquid by coating equipment, drying and rolling to obtain the composite adsorption film, wherein the thickness of the composite adsorption film is 100 mu m.
Comparative example 1
An instant freeze-dried fish gelatin is prepared by the following method:
1) The fish gelatin is placed in a saturated steam environment for 20min to be rehydrated, the rehydrated fish gelatin is transferred into a foaming pool containing 80 ℃ water for foaming treatment, and the mass ratio of the rehydrated fish gelatin to the water is 1:60g/g, the treatment time is 8h; filtering and recycling after the foaming treatment is finished to obtain the foaming fish glue for standby;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow temperature liquid nitrogen freezing treatment, wherein the treatment temperature is-196 ℃, and the treatment time is 20 minutes, so that the frozen fish glue is obtained; and (5) drying the frozen fish gelatin for 30 hours at 40 ℃ to obtain the frozen fish gelatin, and vacuum packaging to obtain the instant frozen fish gelatin.
Test example 1
Sensory evaluation was performed on the instant freeze-dried fish gelatin prepared in part of the representative examples and comparative examples of the present invention, for detecting the fishy smell degree of the instant freeze-dried fish gelatin under different processes. The panelists were trained according to the method provided in GB/T15549-2022 sensory analysis methodology for detecting and identifying odor aspects by entry and training of the panelists. 30 evaluators required by compound training are selected, and the fishy smell of the instant freeze-dried fish gelatin is scored; the grading standard is made of ten kinds, the intensity of the fishy smell is reflected by 1-10, and the higher the grading is, the stronger the fishy smell is represented; wherein, 1 represents no fishy smell, and 10 represents the fishy smell of the same batch of fishy glue raw materials which are not subjected to any treatment; the environmental temperature of sensory evaluation is 25 ℃, the relative humidity is 50%, each group is scored three times, and the rest is carried out for 30 minutes between each round; the result is an arithmetic average, retaining a decimal place. The fish smell sensory evaluation results of the instant freeze-dried fish gelatin are shown in table 1.
Table 1:
| name of the name | Sensory evaluation score |
| Example 1 | 1.9 |
| Example 3 | 2.7 |
| Example 4 | 1.7 |
| Example 5 | 4.1 |
| Example 6 | 6.7 |
| Comparative example 1 | 7.9 |
As can be seen from the evaluation results of table 1, the fishy smell removing effect of the prepared composite adsorption film on the fish gelatin increases gradually along with the increase of the content of the polymerization product and the polyvinyl chloride in the casting film liquid within the scope of the invention, and example 4 has the best fishy smell removing effect, but the fishy smell removing degree is limited relative to examples 1 and 3, so the ratio of example 1 is preferred in practical application. In example 5, the adsorption film obtained by directly combining bentonite and polyvinyl chloride had an effect superior to that of the polyvinyl chloride film, but the effect was inferior to that of example 1 due to problems of dispersion of bentonite, insufficient hydrophilicity of polyvinyl chloride, and the like. The fishy smell was the strongest in comparative example 1 without the deodorization treatment.
The reason for this is probably that the present invention employs polyvinyl chloride, which enhances the immobilization of the organic amine by the adsorption film by quaternization based on the reactivity of the carbon-chlorine bond. The hydrophilicity of the polyvinyl chloride film is insufficient, so that the bentonite-based polymer material is used for assisting the polyvinyl chloride film to form a porous structure, and the hydrophilicity, roughness and porosity of the film are further improved; the hydroxyl bentonite reacts with 4-amino-3, 3-dimethylbutyl trimethoxy silane and 2-bromohexanoyl bromide, and then is polymerized with 3-methyl-3-butenamide and triethylene glycol diacrylate, and the alkyl branched structure and ether oxygen bond are beneficial to improving the dispersibility among particles of a polymerization product, preventing the agglomeration of bentonite and forming a loose microstructure. The composite adsorption film prepared by the solution casting method has good hydrophilicity and microscopic pores, can improve the surface roughness of the film, is more effectively combined with water in a foaming pool and adsorbs fishy smell substances, and achieves the aim of removing fishy smell.
Test example 2
The rehydration rate of the instant freeze-dried fish gelatin prepared by the partial representative embodiment of the invention is tested, so that the foaming performance of the instant freeze-dried fish gelatin in eating is reflected. The quality of dried products of the instant freeze-dried fish gelatin in different embodiments is recorded respectively, then the instant freeze-dried fish gelatin is placed in a steaming rack, the instant freeze-dried fish gelatin is steamed for 30min under normal pressure by adopting a conventional rehydration means, the steamed and rehydrated instant freeze-dried fish gelatin is drained until no water drops, and the drained quality after rehydration is recorded.
Each group was tested 3 times and the results were arithmetically averaged. The test results of the rehydration rate of the instant freeze-dried fish gelatin are shown in table 2.
Table 2:
| name of the name | Rehydration Rate (%) |
| Example 1 | 427 |
| Example 2 | 409 |
| Example 3 | 420 |
| Example 4 | 438 |
As can be seen from the test results in Table 2, the instant freeze-dried fish gelatin has a rehydration rate of more than 300%, good rehydration performance and is convenient and quick to eat.
Claims (10)
1. The preparation method of the instant freeze-dried fish gelatin comprises the steps of rehydration, foaming treatment, deodorization treatment, ultralow-temperature liquid nitrogen freezing, freeze-drying and drying of the fish gelatin, and is characterized in that: the freezing adopts ultralow-temperature liquid nitrogen for freezing; the fishy smell removing treatment adopts a composite adsorption film to adsorb fishy smell substances; the composite adsorption film is prepared by firstly treating bentonite with alkali liquor to introduce hydroxyl and obtain hydroxyl bentonite, then carrying out a coupling reaction on the hydroxyl bentonite and 4-amino-3, 3-dimethylbutyl trimethoxy silane, subsequently carrying out a coupling reaction on the coupling product and 2-bromohexanoyl bromide, forming an amide bond through substitution of bromine atoms of acyl bromide groups to connect, polymerizing the obtained amidated product with 3-methyl-3-butenamide and triethylene glycol diacrylate under catalysis to obtain a polymerization product, mixing the polymerization product, polyvinyl chloride and a solvent to prepare a casting film liquid, and preparing the composite adsorption film by a solution casting film method.
2. The method for preparing instant freeze-dried fish gelatin according to claim 1, comprising the steps of:
1) The fish gelatin is placed in a saturated steam environment for 10-30 min for rehydration, the rehydrated fish gelatin is transferred into a foaming pool containing 75-90 ℃ water for foaming treatment, a composite adsorption film is adopted for deodorization treatment in the foaming treatment process, and the foaming treatment is finished and filtered and recovered to obtain the foaming fish gelatin for later use;
2) The foaming fish glue is subjected to water washing, impurity removal and slicing, and then is transferred to liquid nitrogen freezing equipment for ultralow-temperature liquid nitrogen freezing treatment to obtain frozen fish glue; and drying the frozen fish gelatin to obtain the freeze-dried fish gelatin, and vacuum packaging to obtain the instant freeze-dried fish gelatin.
3. The method for preparing instant freeze-dried fish gelatin according to claim 2, wherein: in the foaming treatment in the step 1), the mass ratio of the fish gelatin to water after rehydration is 1: (45-70) g/g, and the treatment time is 4-10 h; in the deodorization treatment, the ratio of the film width of the composite adsorption film to the bottom area of the foaming pool is 0.2-0.5 m:1m 2 The height of the composite adsorption film is equal to the water depth of the foaming pool.
4. The method for preparing instant freeze-dried fish gelatin according to claim 2, wherein: the temperature of the ultralow temperature liquid nitrogen freezing treatment in the step 2) is-210 to-196 ℃, and the treatment time is 10-30 min.
5. The method for preparing instant freeze-dried fish gelatin according to claim 2, wherein the preparation method of the composite adsorption film comprises the following steps in parts by weight:
s1, uniformly mixing 2.55-3.60 parts of bentonite with 45-60 parts of sodium hydroxide aqueous solution, heating, performing heat treatment, centrifuging, collecting precipitate, washing the precipitate until eluent is neutral, and drying to obtain hydroxyl bentonite for later use;
s2, taking 2.75-3.70 parts of the hydroxyl bentonite and 100-150 parts of toluene, uniformly mixing, adding 2.20-2.95 parts of 4-amino-3, 3-dimethylbutyl trimethoxy silane under the protection of nitrogen, and then carrying out coupling reaction under the condition of reflux; after the coupling reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate until the eluent is neutral, and drying to obtain a coupling product for later use;
s3, taking 2.15-2.80 parts of the coupling product, 3.15-4.05 parts of triethylamine and 60-90 parts of toluene, uniformly mixing, adding 3.85-5.00 parts of 2-bromohexanoyl bromide, and carrying out amidation reaction; after the amidation reaction is finished, collecting the precipitate through centrifugal separation, washing the precipitate with acetone at 0-4 ℃, and drying to obtain an amidation product for later use;
under the protection of S4 and nitrogen, 2.45 to 3.45 parts of amidated products, 1.70 to 2.40 parts of 2,2' -bipyridine, 0.75 to 1.05 parts of cuprous bromide and 125 to 175 parts of N, N-dimethylformamide are taken, evenly mixed, and after the color of the mixed solution turns into dark brown, 4.40 to 6.15 parts of 3-methyl-3-butenamide and 0.65 to 0.90 part of triethylene glycol diacrylate are added for polymerization reaction; filtering and collecting a filter cake after the polymerization reaction is finished, washing the filter cake by acetone at 0-4 ℃ and drying to obtain a polymerization product for later use;
s5, mixing the polymerization product, polyvinyl chloride and N, N-dimethylacetamide in proportion, uniformly dispersing the components after heating and melting, and degassing to obtain a casting solution; casting the casting solution on a substrate, uniformly coating by coating equipment, drying and rolling to obtain the composite adsorption film.
6. The method for preparing instant freeze-dried fish gelatin according to claim 5, wherein: the concentration of the sodium hydroxide aqueous solution in the step S1 is 0.5-1.0 mol/L.
7. The method for preparing instant freeze-dried fish gelatin according to claim 5, wherein: the temperature of the heat treatment in the step S1 is 40-65 ℃ and the treatment time is 0.5-2 h; the temperature of the coupling reaction in the step S2 is 110-125 ℃, and the reaction time is 12-24 hours; the amidation reaction temperature in the step S3 is 0-15 ℃ and the reaction time is 6-18 h; the temperature of the polymerization reaction in the step S4 is 55-70 ℃ and the reaction time is 3-8 h.
8. The method for preparing instant freeze-dried fish gelatin according to claim 5, wherein the casting solution in step S5 comprises the following components in percentage by mass: 0.15 to 1.80 weight percent of polymerization product, 10.5 to 15.0 weight percent of polyvinyl chloride and the balance of N, N-dimethylacetamide.
9. The method for preparing instant freeze-dried fish gelatin according to claim 5, wherein: in the step S5, the polyvinyl chloride is in a film grade; the thickness of the composite adsorption film is 50-200 mu m.
10. An instant freeze-dried fish gelatin, characterized in that it is prepared by the method according to any one of claims 1 to 9.
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| CN116686957B (en) * | 2023-07-13 | 2024-01-30 | 广东官栈营养健康科技有限公司 | Preparation method of bubble-free dry flower adhesive |
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