CN101921547A - Method for pretreating gelatin by liming - Google Patents

Method for pretreating gelatin by liming Download PDF

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CN101921547A
CN101921547A CN2010102642404A CN201010264240A CN101921547A CN 101921547 A CN101921547 A CN 101921547A CN 2010102642404 A CN2010102642404 A CN 2010102642404A CN 201010264240 A CN201010264240 A CN 201010264240A CN 101921547 A CN101921547 A CN 101921547A
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ossein
liming
gelatin
hours
pickling
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CN101921547B (en
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魏连波
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Anhui Bbca Group Co ltd
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Bengbu Fengyuan Gelatin Co Ltd
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Abstract

The invention provides a method for pretreating gelatin by liming. The grease content of a gelatin finished product can be reduced by treating pickled and rinsed ossein with dilute ammonia water. The ammonia water is used to replace sodium hydroxide, a saponified matter formed after a reaction and emulsified particles formed by the saponified matter and fat have high solubility and can be separated from the ossein easily, and the residual fat content of the ossein is low. The method can reduce the grease content of the gelatin finished product, improve the liming efficiency of the gelatin and shorten the liming circle of the gelatin.

Description

The pretreated method of a kind of gelatin by liming
Technical field
The present invention relates to the gelatin technology of preparing, be specifically related to the liming pretreatment process that alkaline process prepares gelatin.
Background technology
Gelatin (gelatin) is a kind of water soluble protein mixture, generally by the collagen in animal bone, ligament, the tendon etc. through acid or alkali partial hydrolysis or in water, boil and produce, crisp or meal shape that colourless or little Huang is transparent, swelling forms gel (moisture for conducting oneself with dignity 5~10 times) in 35~40 ℃ of water.Be widely used in food and make tamanori, photographic film, spectral filter etc.
At present gelatin generally adopts the alkaline process preparation, generally comprises pickling, washing, liming, puies forward step such as glue.
Mineral substance in the aggregate mainly is that some are water-fast, and is dissolved in calcium, magnesium phosphoric acid salt and the carbonate of acid, accounts for 60~65% of total amount, wherein calcium phosphate Ca 3(PO 4) 2Account for 85% of total mineral, lime carbonate CaCO 3Account for 10% of total mineral.With hydrochloric acid the dissolving of aggregate mineral is removed, the organic substance that dissociates simultaneously and mainly form by ossein, i.e. " ossein ", this process is called pickling.Reaction formula is as follows:
Ca 3(PO 4) 2+4HCl=2CaCl 2+Ca(H 2PO 4) 2
CaCO 3+2HCl=CaCl 2+H 2O+CO 2
The alkaline purification process of soaking raw material with milk of lime becomes " liming ".Liming is the very important ring of alkaline process glue, and raw material is under the effect of alkali, and the tissue of the raw material that can not only loosen, and can dissolve and remove the organism that those influence the gelatin quality is as soluble proteins, pigment etc.The initial rubber protofibril water-swelling of handling through liming, loosen, open, internal bond strength weakens, and cuts off easily, helps the stripping of collagen protein.
In traditional preparation method, usually the ossein after the pickling washing is carried out the liming pre-treatment with caustic soda to ossein before liming, promptly in the qualified pickling ossein of washing, add about 0.5% the lipid acid of rare caustic soda soln, thereby reach the purpose that reduces fat content in the gelatin to remove fat residual in the ossein and to go out by steatolysis.
Yet because the fat and the lipid acid that contain in the pickling ossein mostly are unsaturated fatty acids greatly, the solubleness saponified and and adipogenic emulsified particle saponified by this that forms with caustic soda reaction back is low, is difficult to separate the residual fat quantity height of ossein with ossein; The residual fat quantity height of ossein can very easily generate the lower fatty acid calcium of solubleness with lime reaction in following road liming process, stop up the ossein pore, influences the infiltration of calcium hydroxide to ossein inside, and then influences the effect of liming.Because caustic soda is a highly basic, in the process of degreasing ossein is shunk significantly in addition, the capillary porosity duct in the ossein diminishes, and influences that calcium hydroxide influences the effect of liming to the infiltration of ossein inside in next step liming process.Under identical conditions, make the cycle stretch-out of liming.
Summary of the invention
The object of the present invention is to provide the pretreated method of a kind of gelatin by liming.
Gelatin by liming pretreatment process of the present invention is that the ossein after the pickling washing is handled with weak ammonia, to be used for reducing the fat content of gelatin finished product.
Specifically comprise the steps:
1) in the pickling ossein after washing, adds 3~5% dilute ammonia solution, agitate, make ossein and solution uniform mixing, reacted 24~48 hours, in the process of reacting, agitated once with pressurized air in per 2~4 hours with pressurized air;
2) after reaction finishes, put raffinate, wash 2~4 times, reacted ossein is called G1;
3) 3~5% dilute ammonia solution and 0.5~1% hydrogen peroxide solution were mixed by 1: 1 be made into mixed solution;
4) mixed solution is added react 24~48 hours among the G1, in the process of reaction, agitated once with pressurized air in per 2~4 hours;
5) after reaction finishes, put raffinate, wash 2~4 times, reacted ossein is called G2.
Above-mentioned steps 1) the pickling ossein is 3.6~4.0 to get final product through being washed to the pH value.Can be by repeating above-mentioned steps 4) and 5) 1~3 time, with the reinforcement degreasing effect.
The present invention's aqueous ammonia to replace caustic soda, the solubleness saponified and and adipogenic emulsified particle saponified by this that the reaction back forms is higher, and easily separated with ossein, the residual fat quantity of ossein is few.The inventive method can reduce the fat content of gelatin finished product, improves the liming efficient of gelatin, shortens the liming cycle.
Embodiment
Following examples further specify content of the present invention, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, modification or replacement to the inventive method, step or condition are done all belong to scope of the present invention.
If do not specialize the conventional means that used technique means is well known to those skilled in the art among the embodiment.
Embodiment 1 gelatin by liming pre-treatment
1, pickling and washing
Pickling and washing can be carried out according to existing ordinary method.Particularly, aggregate being processed into the skeletal grain that particle diameter is 10~15mm, is that 4% hydrochloric acid flows and soaks with concentration, and the hydrochloric acid content that skeletal grain per ton per hour passes through is 400L.When the concentration of hydrochloric acid that soaks remains unchanged (96h), reach the stage of stable development, and keep 24 hours stages of stable development, detect mineral substance and take off substantially to the greatest extent, aggregate is softer and flexible.Wash with water to pH>3.5.
2, liming pre-treatment
The dilute ammonia solution of adding 3% is agitated with pressurized air in the qualified pickling ossein (being washed to pH3.6) of washing, makes ossein and solution uniform mixing, reacts 24 hours.Agitated once with pressurized air in per 2 hours.Reaction is put raffinate after finishing, and washes 2 times.Reacted ossein is called G1.Dilute ammonia solution with 3% and 0.5% hydrogen peroxide solution are made into mixed solution and added among the G1 reaction 24 hours by mixing at 1: 1, agitate once with pressurized air in per 2 hours.Reaction is put raffinate after finishing, and washes 2 times.Reacted ossein is called G2.By this program ossein and mixed solution are reacted 2 times, the liming pre-treatment of washing back finishes.
Embodiment 2 gelatin by liming pre-treatment
The dilute ammonia solution of adding 4% is agitated with pressurized air in the qualified ossein pH3.8 of washing, makes ossein and solution uniform mixing, reacts 36 hours.Agitated once with pressurized air in per 3 hours.Reaction is put raffinate after finishing, and washes 3 times.Reacted ossein is called G1.Dilute ammonia solution with 4% and 0.8% hydrogen peroxide solution are made into mixed solution and added among the G1 reaction 36 hours by mixing at 1: 1, agitate once with pressurized air in per 3 hours.Reaction is put raffinate after finishing, and washes 3 times.Reacted ossein is called G2.By this program ossein and mixed solution are reacted 3 times, the liming pre-treatment of washing back finishes.
Embodiment 3 gelatin by liming pre-treatment
The dilute ammonia solution of adding 5% is agitated with pressurized air in the qualified ossein pH4.0 of washing, makes ossein and solution uniform mixing, reacts 48 hours.Agitated once with pressurized air in per 4 hours.Reaction is put raffinate after finishing, and washes 4 times.Reacted ossein is called G1.Dilute ammonia solution with 5% and 1% hydrogen peroxide solution are made into mixed solution and added among the G1 reaction 48 hours by mixing at 1: 1, agitate once with pressurized air in per 4 hours.Reaction is put raffinate after finishing, and washes 4 times.Reacted ossein is called G2.By this program ossein and mixed solution are reacted 4 times, the liming pre-treatment of washing back finishes.
The comparison of embodiment 4 liming pretreatment processs of the present invention and prior art
Present method is to get 20 kilograms in the same pond pickling material (pig bone) that pickling handles well from the pickling pond of suitability for industrialized production, is equally divided into two parts, and portion is the A sample; Another part is the B sample.The A sample is with rare NaOH pre-treatment, and treatment process is identical with former method; The comparison of two kinds of pretreatment processs is carried out in present method pre-treatment of B sample.The pre-treatment of two kinds of methods finishes back (stirring identical number of times, 48 hours identical treatment times), surveys the oil length of ossein, and the ossein oil length of A sample is 1.0~1.05%; The ossein oil length of B sample is 0.43~0.5%.
A sample, B sample add 3% milk of lime simultaneously through pretreated ossein to carry out liming and handles, and treats that the liming cycle reaches the following glue speed (50 ℃, 2 hours ossein is hydrolyzed into the amount of gelatin) that begins to survey the liming ossein after 45 days.Surveyed in per 5 days and once play glue speed.Just can reach when being 50 days and produce glue requirement (50 ℃, the amount that 2 hours ossein is hydrolyzed into gelatin is 50 grams) with the pretreated ossein liming cycle of present method; And with the pretreated ossein of caustic soda under identical liming condition, the liming cycle will be more than 60 days, its down glue speed just can reach and produce the glue requirement.
Table 1 present method pretreating effect table
Figure BSA00000246731300051
Annotate:
(1), the detection method of following glue speed:
Get 1 kilogram in A sample (after the liming), B sample (after the liming) respectively, add water washing 2~3 times, till water is clear, and then put into two identical sieve baskets, draining 30 minutes respectively; Weigh style 500 grams behind the draining, put into the large beaker of 2000ml, add 70 ℃ of hot deionized water 1000ml, put into water-bath and adjust temperature to 50 ℃, be incubated under 50 ℃ and pick up counting.After 2 hours, the glue in the beaker is drained, surveys the volume (ml) and the concentration (%) of glue, be converted to down glue speed according to following formula:
W=V×d×x%
The following glue speed of W-glue (2 hours following glue amount of glue), g/h;
The volume of V-glue, ml;
The weight percentage of x%-glue, %;
The proportion of d-glue (50 ℃), g/ml;
(2), the measuring method of ossein residual oil content:
1. principle:
By in the benzene extraction degreasing ossein residual grease, calculate oil length.
2. instrument and reagent:
-thermostatic drying chamber;
-Soxhlet oil extractor 300W electric furnace;
-purified petroleum benzin;
-round-bottomed flask.
3. measure:
Sample thief 1000 grams, putting into baking oven dries to constant weight, pulverize by two layers of (upper strata 6 order with hand hammer, lower floor's 10 orders) screen, on, following two does not take by weighing middle sample 15 grams, tie the Soxhlet oil extractor of putting into bottle weight of the known end with filter paper, logical water coolant adds about purified petroleum benzin 120ml, in round-bottomed flask, connects power supply and progressively is elevated to the purified petroleum benzin circulation well by low temperature, extracted 4 hours, cut off the electricity supply, take out the sample bag after a while, reclaiming purified petroleum benzin only has 5ml benzene oil mixt in the bottle on earth, take off end bottle and put into 105 ± 5 ℃ of thermostatic drying chambers, dry by the fire to take out in 2 hours and put into moisture eliminator, be chilled to room temperature, weigh.
4. calculate:
Figure BSA00000246731300061
In the formula: m 1-oil and end bottle weight (gram);
m 2-empty end bottle weight (gram);
M-example weight (gram).
5. permissible error:
Twice replicate(determination) value differs and is no more than 0.3%.

Claims (4)

1. gelatin by liming pretreatment process, it is before liming the ossein after the pickling washing to be handled with weak ammonia.
2. the method for claim 1, it comprises the steps:
1) in the pickling ossein after washing, adds 3~5% dilute ammonia solution, agitate, make ossein and solution uniform mixing, reacted 24~48 hours, in the process of reacting, agitated once with pressurized air in per 2~4 hours with pressurized air;
2) after reaction finishes, put raffinate, wash 2~4 times, reacted ossein is called G1;
3) 3~5% dilute ammonia solution and 0.5~1% hydrogen peroxide solution were mixed by 1: 1 be made into mixed solution;
4) mixed solution is added react 24~48 hours among the G1, in the process of reaction, agitated once with pressurized air in per 2~4 hours;
5) after reaction finishes, put raffinate, wash 2~4 times, reacted ossein is called G2.
3. method as claimed in claim 2 is characterized in that, wherein the pH of the pickling ossein of step 1) after washing is 3.6~4.0.
4. as claim 2 or 3 described methods, it is characterized in that, also comprise repeating step 4) and 5) 1~3 time.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB406018A (en) * 1932-08-12 1934-02-12 Miles Andrew Corbett Improvements in or relating to the treatment of mineral sand for the separation of one constituent therein from another
GB831124A (en) * 1955-05-18 1960-03-23 Alfred Bloch Purification of collagen
RU2021991C1 (en) * 1992-11-19 1994-10-30 Владислав Григорьевич Завальный Method of raw decalcification in gelatin production
CN1318607A (en) * 2000-04-19 2001-10-24 包头东宝乐凯明胶有限公司 Technological process of producing bone gelatine for color photography

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB406018A (en) * 1932-08-12 1934-02-12 Miles Andrew Corbett Improvements in or relating to the treatment of mineral sand for the separation of one constituent therein from another
GB831124A (en) * 1955-05-18 1960-03-23 Alfred Bloch Purification of collagen
RU2021991C1 (en) * 1992-11-19 1994-10-30 Владислав Григорьевич Завальный Method of raw decalcification in gelatin production
CN1318607A (en) * 2000-04-19 2001-10-24 包头东宝乐凯明胶有限公司 Technological process of producing bone gelatine for color photography

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
周世海: "骨明胶生产", 《明胶科学与技术》 *
邓文: "骨明胶生产中的预浸灰工艺", 《明胶科学与技术》 *

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Denomination of invention: A method for pre-treatment of gelatin by soaking in ash

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