CN109554120B - Method for producing oxhide gelatin by alkaline process - Google Patents
Method for producing oxhide gelatin by alkaline process Download PDFInfo
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- CN109554120B CN109554120B CN201811441992.6A CN201811441992A CN109554120B CN 109554120 B CN109554120 B CN 109554120B CN 201811441992 A CN201811441992 A CN 201811441992A CN 109554120 B CN109554120 B CN 109554120B
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- 239000008273 gelatin Substances 0.000 title claims abstract description 68
- 229920000159 gelatin Polymers 0.000 title claims abstract description 68
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 68
- 108010010803 Gelatin Proteins 0.000 title claims abstract description 67
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 106
- 238000005406 washing Methods 0.000 claims abstract description 47
- 238000007710 freezing Methods 0.000 claims abstract description 43
- 230000008014 freezing Effects 0.000 claims abstract description 43
- 238000000605 extraction Methods 0.000 claims abstract description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 230000001954 sterilising effect Effects 0.000 claims abstract description 13
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 8
- 238000005554 pickling Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 3
- 239000003292 glue Substances 0.000 claims description 170
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 238000009835 boiling Methods 0.000 claims description 45
- 238000002791 soaking Methods 0.000 claims description 40
- 239000010985 leather Substances 0.000 claims description 31
- 239000000499 gel Substances 0.000 claims description 23
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 21
- 239000000920 calcium hydroxide Substances 0.000 claims description 21
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 20
- 239000000725 suspension Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001728 nano-filtration Methods 0.000 claims description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 2
- 239000001828 Gelatine Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004026 adhesive bonding Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013611 frozen food Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000003041 ligament Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 210000004885 white matter Anatomy 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09H—PREPARATION OF GLUE OR GELATINE
- C09H3/00—Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention discloses a method for producing oxhide gelatin by an alkaline process, and belongs to the technical field of gelatin processing. The method comprises the steps of raw material pretreatment, alkali pretreatment, water washing and freezing, liming, washing and pickling, acid removal and neutralization, gelatin extraction, filtering, concentration, high-temperature sterilization and drying, wherein sodium chloride solution treatment is added in the pretreatment, and the breakage of chemical bonds in cowhide is accelerated through the alkali pretreatment process before liming, so that the liming process is accelerated, the gelatin production time is shortened, the freezing operation is carried out before the liming operation and in the operation process to ensure that the structure of the prepared gelatin is more complete, the gelatin extraction efficiency is increased through four times of gelatin extraction operations in the extraction process, and the gelatin strength and viscosity are effectively improved through the freezing operation in the gelatin extraction process.
Description
Technical Field
The invention relates to a method for producing oxhide gelatin by an alkaline process, and belongs to the technical field of gelatin processing.
Background
Gelatin (Gelatin) is a high polymer of high molecular polypeptides obtained by purifying and primarily hydrolyzing collagen contained in animal skin, bone, cartilage, ligament, and muscle membrane, and is also called animal Gelatin and fat glue. The gelatin finished product is a colorless or light yellow, transparent or semitransparent and hard amorphous substance, and the white matter quantity is better. The gelatin is insoluble in cold water, but can slowly absorb water to swell and soften, and the gelatin can absorb 5-10 times of water by weight. Gelatin belongs to a macromolecular hydrophilic colloid, is a low-calorie health food with higher nutritive value, can be used for making candy additives, frozen food additives and the like, and is an indispensable raw material in the aspects of photographic films, X-ray films, aviation films, artificial board adhesives, belt adhesives, rubber products, cotton cloth, papermaking and the like in industry.
In the prior art, five methods of producing gelatin mainly comprise an alkaline method, an acid salt method, a salt-alkali method and an enzyme method, and the most common production methods in industrial production at present are the alkaline method and the acid method, wherein the alkaline method is used for producing more than half of gelatin in the market, and the alkaline method can be used for preparing the high-viscosity gelatin, but the extraction efficiency is low, and the production process takes long time, which can be as long as 35-90 days, so that the method for improving the gelatin extraction rate of the alkaline production process and reducing the production period is very important to find.
Disclosure of Invention
In order to solve the problems, the invention provides a method for producing gelatin by an alkaline method, which increases sodium chloride solution treatment in pretreatment and accelerates the breakage of chemical bonds in cowhide through an alkaline pretreatment process before liming, thereby accelerating the liming process and shortening the time for producing gelatin.
The technical scheme of the invention is to provide a method for producing gelatin by an alkaline method, which comprises the steps of raw material pretreatment, alkaline pretreatment, washing and freezing, liming, washing and pickling, acid removal and neutralization, gelatin extraction, filtration, concentration, high-temperature sterilization and drying, and the method comprises the following specific steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.4-0.8% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.2-2.0% sodium chloride solution at 40-50 deg.C for 3-6 hr, and washing with water to remove sodium chloride;
(2) alkali pretreatment: adding sodium hydroxide in an amount of 0.4-0.6 wt% of cow leather, adding water to control the concentration of sodium hydroxide solution to 0.6-0.7 wt%, and soaking at 40-50 deg.C for 10-14 hr; separating alkali liquor and cow leather after reaction;
(3) washing with water and freezing: washing the residual alkali liquor of the cow leather by using water, and freezing the cow leather to-5 to-10 ℃;
(4) liming: soaking the frozen cowhide obtained in the step (3) in a calcium hydroxide suspension with the mass concentration of 0.5-3%, wherein the weight ratio of the cowhide to the calcium hydroxide suspension is 1: (2-3) soaking for 1-2d, performing ash replacement operation, removing the old calcium hydroxide suspension, cleaning cow leather with clear water, freezing the cow leather to-5 to-10 ℃, and soaking for 4-8d with the calcium hydroxide suspension with the mass concentration of 0.5-3%;
(5) washing and pickling: washing the soaked cowhide with water until the pH value of the washing water reaches 8.0-8.5, adding water to immerse the raw materials, adding hydrochloric acid to adjust the pH value to 4.0-4.5, and soaking for 10-15 h;
(6) acid-removing neutralization: washing with water to remove acid, adding sodium hydroxide solution, soaking for 3-4 hr, and washing with water until pH is 5.5-6.0 before extracting gel;
(7) extracting glue: the method comprises four operations:
primary gum extraction: adding the prepared material treated in the step (6) into a glue boiling pot, adding water with the water temperature of 20-30 ℃ into the glue boiling pot in advance, ensuring that the prepared material is completely immersed in warm water, slowly heating to 45-55 ℃, discharging glue liquid when the glue boiling time reaches 4.5-5 hours, and freezing the glue liquid to-1-5 ℃;
secondary gum extraction: adding warm water of 30-37 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 52-60 ℃, discharging glue liquid when the glue boiling time reaches 5-5.5h, and freezing the glue liquid to-1 to-5 ℃;
and (3) extracting the glue for three times: adding warm water of 40-45 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 60-70 ℃, discharging glue liquid when the glue boiling time reaches 5-5.5h, and freezing the glue liquid to-1 to-5 ℃;
and (4) extracting the glue for four times: adding warm water of 55-65 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 75-85 ℃, and discharging glue solution when the glue boiling time reaches 6-7 hours;
(8) and (3) filtering: thawing frozen glue solution obtained by extracting glue for the first, second and third times at normal temperature, adding 0.5-0.8% W/V (g/mL, the same below) of active carbon or diatomite into the glue solution obtained by extracting glue for the fourth time, stirring for 2.5-3.5h, and filtering to obtain dilute glue solution;
(9) concentration: adding hydrochloric acid solution into the obtained dilute glue solution to adjust the pH of the dilute glue solution to 5.0-6.5, then performing membrane concentration to obtain a concentrated glue solution with the concentration of 28-32%, and sequentially performing membrane concentration by using an ultrafiltration membrane filter cartridge and a nanofiltration membrane filter cartridge, wherein the concentration temperature is 55-65 ℃ and the pressure is 0.2-0.5 MPa;
(10) and (5) glue steaming and sterilization: adding the concentrated glue solution into a three-effect flash evaporator for steam sterilization, wherein the flash evaporation temperature is 140-145 ℃;
(11) extruding and drying: and (3) cooling the flash-evaporated thick glue solution in an aseptic environment, extruding the thick glue solution into glue strips, drying, and crushing to obtain the product.
In one embodiment of the invention, the liming temperature in step (4) is less than 15 ℃.
In one embodiment of the present invention, the pH in step (9) is preferably 5.0 to 5.5.
In one embodiment of the present invention, the pH in step (9) is preferably 5.0 to 5.5.
In one embodiment of the present invention, the temperature of the freezing in step (3) is-8 to-10 ℃.
In one embodiment of the present invention, the pH before the gel extraction in step (6) is 5.8.
The invention has the following technical effects:
(1) the method carries out the alkali pretreatment step before liming, utilizes strong alkali pretreatment, can promote the penetration of the calcium hydroxide alkali liquor in the subsequent liming step, can greatly shorten the liming treatment time and procedure, can finish the liming step only by 5-10 days, and can obviously shorten the process flow compared with the prior art with more than 30 days;
(2) the invention carries out freezing operation on the cowhide before liming and ash changing, the operation step can improve the extraction rate of the gelatin, the extraction rate of the gelatin can reach 86.2 percent, the gel strength and the freezing force can be obviously improved,
(3) the invention also adds freezing operation in the process of extracting the gelatin, and can obviously improve the gel strength and viscosity of the oxhide gelatin through freezing and thawing operation, and the gel strength and viscosity can reach 397g and 5.8 mPa.s.
Detailed Description
And (3) measuring the gel strength: taking 6.67g of gelatin obtained in the extraction, adding 70mL of water, standing at about 20 ℃ for 2h to make the gelatin absorb water and expand, then placing in a water bath at 60 ℃ for 15min to dissolve the gelatin into uniform liquid, and adding water to prepare a glue solution with the mass percentage concentration of 6.67%; covering, placing for 1-4 h, stirring and heating in a water bath at 65 +/-2 ℃ for 15min to uniformly dissolve the sample, placing for 15min at room temperature, horizontally placing the frozen bottle in a constant-temperature water bath at 10 +/-0.1 ℃, sealing with a rubber plug, keeping the temperature for 17 +/-1 h, quickly moving out the frozen bottle, wiping the outer wall, and placing on a test board of a frozen instrument for testing to obtain the gel strength of the gelatin.
And (3) viscosity measurement: : preparing 100mL of glue solution with the mass concentration of 6.67% from the extracted gelatin in a triangular flask, cooling the glue solution to about 61 ℃, starting a super constant-temperature water bath to ensure that the temperature of the glue solution flowing through a viscometer jacket is 60 +/-0.1 ℃, blocking the tail end of a capillary tube of a Boehringer viscometer to prevent air or bubbles from entering, and quickly pouring the glue solution into a viscosity tube until the glue solution exceeds the upper scale mark by 2-3 cm. And (3) inserting a thermometer into the viscometer, adjusting the level of the glue solution to the upper scale mark when the temperature is stabilized at 60 +/-0.1 ℃, starting timing when the tail end of the capillary is released, stopping timing when the level of the glue solution reaches the lower scale mark, and recording the time as t seconds.
By the viscosity calculation formula: n-1.005 At-1.005B/t, the viscosity of the glue solution is 6.5 mPa.s, which reaches the standard of medicinal gelatin, wherein n-glue solution viscosity, mPa.s, t-flow time, s; a, B-viscometer constants.
Gelatin extraction rate MGelatin/MRaw materials×100％。
Example 1
A method for producing gelatin by an alkaline process comprises the following specific steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.5% sodium sulfide solution, unhairing, cutting the cowhide into 5mm × 5mm pieces, soaking in 1.4% sodium chloride solution at 40 deg.C for 5 hr, and washing with water to remove sodium chloride;
(2) alkali pretreatment: adding sodium hydroxide according to 0.5% of cow leather weight, adding water to control the concentration of sodium hydroxide solution to be 0.6 wt%, and soaking at 40 deg.C for 11 h; separating alkali liquor and cow leather after reaction;
(3) washing with water and freezing: washing the residual alkali liquor of cow leather with water, and freezing cow leather to-10 deg.C;
(4) liming: soaking the frozen cow leather obtained in the step (3) in a calcium hydroxide suspension with the concentration of 2%, wherein the weight ratio of the cow leather to the calcium hydroxide suspension is 1: 2, soaking for 1d, performing ash replacement operation, removing the old calcium hydroxide suspension, cleaning cowhide with clear water, freezing the cowhide to-10 ℃, and soaking for 6d with calcium hydroxide suspension with mass concentration of 0.5-3%;
(5) washing and pickling: washing the soaked cowhide with water until the pH value of the washing water reaches 8.0-8.1, adding water to immerse the raw materials, adding hydrochloric acid to adjust the pH value to 4.0-4.1, and soaking for 12 h;
(6) acid-removing neutralization: washing with water to remove acid, adding sodium hydroxide solution, soaking for 3h, and washing with water until pH is 5.5 before extracting gel;
(7) extracting glue: the method comprises four operations:
primary gum extraction: adding the prepared material treated in the step (6) into a glue boiling pot, adding water with the water temperature of 25 ℃ into the glue boiling pot in advance, ensuring that the prepared material is completely immersed in warm water, slowly heating to 45 ℃, discharging glue liquid when the glue boiling time reaches 5 hours, and freezing the glue liquid to-1 ℃;
secondary gum extraction: adding warm water of 35 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 55 ℃, discharging glue solution when the glue boiling time reaches 5 hours, and freezing the glue solution to-1 ℃;
and (3) extracting the glue for three times: adding 45 deg.C warm water into the glue boiling pot again, and ensuring the warm water to be completely immersed, heating slowly to 65 deg.C, discharging glue solution when the glue boiling time reaches 5 hr, and freezing to-1 deg.C;
and (4) extracting the glue for four times: adding warm water of 55 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed in the prepared materials, slowly heating to 75 ℃, and discharging the glue solution when the glue boiling time reaches 6 hours;
(8) and (3) filtering: unfreezing frozen glue solution obtained by the first, second and third glue extraction at normal temperature, adding 0.5% W/V active carbon into the glue solution obtained by the fourth glue extraction, stirring for 2.5h, and filtering to obtain dilute glue solution;
(9) concentration: adding a hydrochloric acid solution into the obtained dilute glue solution to adjust the pH of the dilute glue solution to 5.0, then carrying out membrane concentration to obtain a concentrated glue solution with the concentration of 28%, and sequentially carrying out membrane concentration by using an ultrafiltration membrane filter cartridge and a nanofiltration membrane filter cartridge, wherein the concentration temperature is 55 ℃, and the pressure is 0.3 MPa;
(10) and (5) glue steaming and sterilization: adding the concentrated glue solution into a triple-effect flash evaporator for steam sterilization, wherein the flash evaporation temperature is 142 ℃;
(11) extruding and drying: and (3) cooling the flash-evaporated thick glue solution in an aseptic environment, extruding the thick glue solution into glue strips, drying, and crushing to obtain the product.
Example 2
A method for producing gelatin by an alkaline process comprises the following specific steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.7% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.8% sodium chloride solution at 45 deg.C for 3.5 hr, and washing with water to remove sodium chloride;
(2) alkali pretreatment: adding sodium hydroxide according to 0.6% of the weight of the cowhide, adding water to control the concentration of the sodium hydroxide solution to be 0.7 wt%, and soaking at 50 deg.C for 14 h; separating alkali liquor and cow leather after reaction;
(3) washing with water and freezing: washing the residual alkali liquor of cow leather with water, and freezing cow leather to-7 deg.C;
(4) liming: soaking the frozen cow leather obtained in the step (3) in a calcium hydroxide suspension with the concentration of 2%, wherein the weight ratio of the cow leather to the calcium hydroxide suspension is 1: 2, soaking for 1d, performing ash replacement operation, removing the old calcium hydroxide suspension, cleaning cowhide with clear water, freezing the cowhide to-7 ℃, and soaking for 4.5d with the calcium hydroxide suspension with the mass concentration of 0.5-3%;
(5) washing and pickling: washing the soaked cowhide with water until the pH value of the washing water reaches 8.0-8.1, adding water to immerse the raw materials, adding hydrochloric acid to adjust the pH value to 4.0, and soaking for 13 h;
(6) acid-removing neutralization: washing with water to remove acid, adding sodium hydroxide solution, soaking for 3h, and washing with water until pH is 5.5 before extracting gel;
(7) extracting glue: the method comprises four operations:
primary gum extraction: adding the prepared material treated in the step (6) into a glue boiling pot, adding water with the water temperature of 30 ℃ into the glue boiling pot in advance, ensuring that the prepared material is completely immersed in warm water, slowly heating to 50 ℃, discharging glue solution when the glue boiling time reaches 5 hours, and freezing the glue solution to-2 ℃;
secondary gum extraction: adding warm water of 37 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 60 ℃, discharging glue solution when the glue boiling time reaches 5 hours, and freezing the glue solution to-2 ℃;
and (3) extracting the glue for three times: adding 45 deg.C warm water into the glue boiling pot again, and ensuring the warm water to be completely immersed, heating slowly to 65 deg.C, discharging glue solution when the glue boiling time reaches 5 hr, and freezing to-2 deg.C;
and (4) extracting the glue for four times: adding warm water of 55 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 80 ℃, and discharging glue solution when the glue boiling time reaches 6 hours;
(8) and (3) filtering: unfreezing frozen glue solution obtained by the first, second and third glue extraction at normal temperature, adding 0.5% W/V active carbon or diatomite into the glue solution obtained by the fourth glue extraction, stirring for 3.0h, and filtering to obtain dilute glue solution;
(9) concentration: adding a hydrochloric acid solution into the obtained dilute glue solution to adjust the pH of the dilute glue solution to 5.5, then carrying out membrane concentration to obtain a concentrated glue solution with the concentration of 30%, and sequentially carrying out membrane concentration by using an ultrafiltration membrane filter cartridge and a nanofiltration membrane filter cartridge, wherein the concentration temperature is 55 ℃, and the pressure is 0.3 MPa;
(10) and (5) glue steaming and sterilization: adding the concentrated glue solution into a triple-effect flash evaporator for steam sterilization, wherein the flash evaporation temperature is 140 ℃;
(11) extruding and drying: and (3) cooling the flash-evaporated thick glue solution in an aseptic environment, extruding the thick glue solution into glue strips, drying, and crushing to obtain the product.
Example 3
A method for producing gelatin by an alkaline process comprises the following specific steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.6% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.4% sodium chloride solution at 40 deg.C for 5 hr, and washing with water to remove sodium chloride;
(2) alkali pretreatment: adding sodium hydroxide according to 0.5% of the weight of the cowhide, adding water to control the concentration of the sodium hydroxide solution to be 0.7 wt%, and soaking at 40 deg.C for 13 h; separating alkali liquor and cow leather after reaction;
(3) washing with water and freezing: washing the residual alkali liquor of cow leather with water, and freezing cow leather to-5 deg.C;
(4) liming: soaking the frozen cowhide obtained in the step (3) in a calcium hydroxide suspension with the concentration of 1.5%, wherein the weight ratio of the cowhide to the calcium hydroxide suspension is 1: 3, soaking for 2d, performing ash replacement operation, removing the old calcium hydroxide suspension, cleaning cowhide with clear water, freezing the cowhide to-5 ℃, and soaking for 7d with the calcium hydroxide suspension with the mass concentration of 0.5-3%;
(5) washing and pickling: washing the soaked cowhide with water until the pH value of the washing water reaches 8.4, adding water to immerse the raw materials, adding hydrochloric acid to adjust the pH value to 4.4, and soaking for 15 h;
(6) acid-removing neutralization: washing with water to remove acid, adding sodium hydroxide solution, soaking for 4h, and washing with water until pH is 5.8 before extracting gel;
(7) extracting glue: the method comprises four operations:
primary gum extraction: adding the prepared material treated in the step (6) into a glue boiling pot, adding water with the water temperature of 20 ℃ into the glue boiling pot in advance, ensuring that the prepared material is completely immersed in warm water, slowly heating to 45 ℃, discharging glue liquid when the glue boiling time reaches 4.5 hours, and freezing the glue liquid to-4 ℃;
secondary gum extraction: adding warm water of 30 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 52 ℃, discharging glue solution when the glue boiling time reaches 5 hours, and freezing the glue solution to-3 ℃;
and (3) extracting the glue for three times: adding warm water of 40 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 60 ℃, discharging glue solution when the glue boiling time reaches 5.5 hours, and freezing the glue solution to-4 ℃;
and (4) extracting the glue for four times: adding warm water of 55 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed in the prepared materials, slowly heating to 75 ℃, and discharging the glue solution when the glue boiling time reaches 7 hours;
(8) and (3) filtering: unfreezing frozen glue solution obtained by the first, second and third glue extraction at normal temperature, adding 0.5% W/V active carbon or diatomite into the glue solution obtained by the fourth glue extraction, stirring for 3 hours, and filtering to obtain dilute glue solution;
(9) concentration: adding a hydrochloric acid solution into the obtained dilute glue solution to adjust the pH of the dilute glue solution to 6.0, then carrying out membrane concentration to obtain a concentrated glue solution with the concentration of 30%, and sequentially carrying out membrane concentration by using an ultrafiltration membrane filter cartridge and a nanofiltration membrane filter cartridge, wherein the concentration temperature is 62 ℃, and the pressure is 0.5 MPa;
(10) and (5) glue steaming and sterilization: adding the concentrated glue solution into a three-effect flash evaporator for steam sterilization, wherein the flash evaporation temperature is 143 ℃;
(11) extruding and drying: and (3) cooling the flash-evaporated thick glue solution in an aseptic environment, extruding the thick glue solution into glue strips, drying, and crushing to obtain the product.
The gelatin in the above examples is tested for gel strength and viscosity, and the first gel is taken as an example, the gel strength can reach 397g at most, and the viscosity can reach 5.8 mPas. The results are shown in table 1, where the extraction is the total gelatin extraction, and the gelatin gel strength and gelatin viscosity are both first pass extraction data. The gel strength of the second gluing and the third gluing can reach 365 and 337g respectively, the viscosity of the gelatin can reach 5.3 and 4.9 mPa.s respectively, and the second gluing and the third gluing have good gel property.
Table 1 properties of the gelatin products prepared according to the invention
| Gelatin sample | Extraction rate | Gelatin gel Strength g | Viscosity of gelatin mPa s |
| Example 1 | 85.4％ | 397 | 5.8 |
| Example 2 | 83.5％ | 384 | 5.4 |
| Example 3 | 86.2％ | 391 | 5.7 |
| Comparative example 1 | 65.2％ | 367 | 4.1 |
| Comparative example 2 | 69.9％ | 301 | 3.8 |
| Comparative example 3 | 72.6％ | 235 | 3.2 |
Comparative example 1
In this comparative example, without the alkaline pretreatment of step (2), and the remaining steps were in accordance with the conditions and example 2, a gelatin product was prepared, and the gel strength and viscosity were measured using the first gel as an example, and the results are shown in Table 1.
Comparative example 2
In the comparative example, the cowhide was not frozen in the water-washing freezing step in the step (3) and the liming step in the step (4), and the remaining steps were performed under the same conditions as in example 2 to prepare a gelatin product
Taking the first glue as an example, the gel strength and viscosity were measured, and the results are shown in Table 1.
Comparative example 3
In the comparative example, the extraction process of step (7) was carried out without freezing the gelatin solution, and the remaining steps were performed under the same conditions as in example 2 to prepare a gelatin product, which was measured for gel strength and viscosity using the first gel as an example, and the results are shown in Table 1.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The method for producing the gelatin by the alkaline method is characterized by comprising the following steps of raw material pretreatment, alkaline pretreatment, washing and freezing, liming, washing and pickling, acid removal and neutralization, gelatin extraction, filtering, concentration, high-temperature sterilization and drying, and specifically comprises the following steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.4-0.8% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.2-2.0% sodium chloride solution at 40-50 deg.C for 3-6 hr, and washing with water to remove sodium chloride;
(2) alkali pretreatment: adding sodium hydroxide in an amount of 0.4-0.6 wt% of cow leather, adding water to control the concentration of sodium hydroxide solution to 0.6-0.7 wt%, and soaking at 40-50 deg.C for 10-14 hr; separating alkali liquor and cow leather after reaction;
(3) washing with water and freezing: washing the residual alkali liquor of the cow leather by using water, and freezing the cow leather to-5 to-10 ℃;
(4) liming: soaking the frozen cowhide obtained in the step (3) in a calcium hydroxide suspension with the mass concentration of 0.5-3%, wherein the weight ratio of the cowhide to the calcium hydroxide suspension is 1: (2-3) soaking for 1-2d, performing ash replacement operation, removing the old calcium hydroxide suspension, cleaning cow leather with clear water, freezing the cow leather to-5 to-10 ℃, and soaking for 4-8d with the calcium hydroxide suspension with the mass concentration of 0.5-3%;
(5) washing and pickling: washing the soaked cowhide with water until the pH value of the washing water reaches 8.0-8.5, adding water to immerse the raw materials, adding hydrochloric acid to adjust the pH value to 4.0-4.5, and soaking for 10-15 h;
(6) acid-removing neutralization: washing with water to remove acid, adding sodium hydroxide solution, soaking for 3-4 hr, and washing with water until pH is 5.5-6.0 before extracting gel;
(7) extracting glue: the method comprises four operations:
primary gum extraction: adding the prepared material treated in the step (6) into a glue boiling pot, adding water with the water temperature of 20-30 ℃ into the glue boiling pot in advance, ensuring that the prepared material is completely immersed in warm water, slowly heating to 45-55 ℃, discharging glue liquid when the glue boiling time reaches 4.5-5 hours, and freezing the glue liquid to-1-5 ℃;
secondary gum extraction: adding warm water of 30-37 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 52-60 ℃, discharging glue liquid when the glue boiling time reaches 5-5.5h, and freezing the glue liquid to-1 to-5 ℃;
and (3) extracting the glue for three times: adding warm water of 40-45 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 60-70 ℃, discharging glue liquid when the glue boiling time reaches 5-5.5h, and freezing the glue liquid to-1 to-5 ℃;
and (4) extracting the glue for four times: adding warm water of 55-65 ℃ into the glue boiling pot again, ensuring that the warm water is completely immersed and prepared, slowly heating to 75-85 ℃, and discharging glue solution when the glue boiling time reaches 6-7 hours;
(8) and (3) filtering: unfreezing frozen glue solution obtained by the first, second and third glue extraction at normal temperature, adding 0.5-0.8% g/mL of active carbon or diatomite into the glue solution obtained by the fourth glue extraction, stirring for 2.5-3.5h, and filtering to obtain dilute glue solution;
(9) concentration: adding hydrochloric acid solution into the obtained dilute glue solution to adjust the pH of the dilute glue solution to 5.0-6.5, then performing membrane concentration to obtain a concentrated glue solution with the concentration of 28-32%, and sequentially performing membrane concentration by using an ultrafiltration membrane filter cartridge and a nanofiltration membrane filter cartridge, wherein the concentration temperature is 55-65 ℃ and the pressure is 0.2-0.5 MPa;
(10) and (5) glue steaming and sterilization: adding the concentrated glue solution into a three-effect flash evaporator for steam sterilization, wherein the flash evaporation temperature is 140-145 ℃;
(11) extruding and drying: and (3) cooling the flash-evaporated thick glue solution in an aseptic environment, extruding the thick glue solution into glue strips, drying, and crushing to obtain the product.
2. The alkaline process for the production of gelatin according to claim 1 wherein the liming temperature in step (4) is less than 15 ℃.
3. The alkaline process for producing gelatin according to claim 1, wherein the pH in step (9) is 5.0 to 5.5.
4. The alkaline process for producing gelatin according to claim 2, wherein the pH in step (9) is 5.0 to 5.5.
5. An alkaline process for the production of gelatin according to any of claims 1 to 4 wherein the freezing temperature in step (3) is between-8 and-10 ℃.
6. The alkaline process for producing gelatin according to any of claims 1 to 4, wherein the pH before the extraction in step (6) is 5.8.
7. Gelatin produced by an alkaline process for the production of gelatin according to any of claims 1 to 6.
8. An artificial board adhesive, a belt adhesive, a rubber product, cotton or paper comprising the gelatin of claim 7.
9. Use of the gelatine of claim 7 in the field of adhesives.
10. Use of an alkaline process for the production of gelatin as claimed in any of claims 1 to 6 in the field of gelatin processing.
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| CN112724243B (en) * | 2021-01-14 | 2022-04-08 | 山东恒鑫生物科技有限公司 | Method for producing oxhide gelatin by using pickled raw skin |
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| CN102433075A (en) * | 2011-11-13 | 2012-05-02 | 逯益民 | Method for quickly preparing special gelatin for candies from raw bone meal |
| CN106634623A (en) * | 2016-09-20 | 2017-05-10 | 苏州吉利鼎海洋生物科技有限公司 | Production process for gelatin |
| CN108203566A (en) * | 2016-12-20 | 2018-06-26 | 湖南尔康明胶有限公司 | The technique that a kind of alkaline process prepares pharmagel |
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| CN102433075A (en) * | 2011-11-13 | 2012-05-02 | 逯益民 | Method for quickly preparing special gelatin for candies from raw bone meal |
| CN106634623A (en) * | 2016-09-20 | 2017-05-10 | 苏州吉利鼎海洋生物科技有限公司 | Production process for gelatin |
| CN108203566A (en) * | 2016-12-20 | 2018-06-26 | 湖南尔康明胶有限公司 | The technique that a kind of alkaline process prepares pharmagel |
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Denomination of invention: A method for producing cowhide gelatin by alkaline method Granted publication date: 20210226 Pledgee: Binzhou Zhanhua sub branch of Postal Savings Bank of China Ltd. Pledgor: Shandong Hengxin Biotechnology Co.,Ltd. Registration number: Y2024980002725 |