CN101768216A - Method for producing casein by using leaching method - Google Patents

Abstract

The invention discloses a method for producing casein by using a leaching method, in particular to a method for producing casein the fat of which is removed by leaching through mixed solvent of liquefied butane and propane or petroleum ether with the temperature of 30-60 DEG C or other ether solvents. The method comprises the following steps: taking crude casein as a raw material; adding a certain amount of crude casein into solvent the volume which is 6-10 times the volume of the crude casein; leaching out the fat of the crude casein at normal temperature and a certain pressure (0.3-0.8MPa) by using a supercritical fluid reverse flow mode or a soxhlet extraction principle; adding a certain amount of water in the crude casein the fat of which is removed and then recovering the solvent; then adding 10 percent of NaOH solution and adjusting the pH value of the solution to be 9-11; heating the crude casein to be completely dissolved at the temperature of 50-65 DEG C; and carrying out separation by using a slag tapping separator, acidity, dehydration, granularity and drying to obtain a casein product the fat content of which is less than or equal to 0.3 percent. The invention solves the problem that the fat content of the casein product produced by a mechanical separation method has high content and can reduce the fat content of the casein protein to be lower than 0.3 percent; and the quality of the product is superior to the quality of the product produced by the traditional process.

Description

The method of method for producing casein by using leaching

Technical field

The present invention relates to the grease manufacture field, specifically a kind of is raw material with the milk crude protein (herdsman of Tibetan claims " song draws ") behind the extraction butter, utilize solvent (main component: the mixture of liquefied butane and propane No. 4, this solvent composition boiling point is mostly below 0 ℃, propane boiling point wherein :-42.07 ℃, butane boiling point :-0.5 ℃, be gas at normal temperatures and pressures, pressurization back be liquid) or the method for No. 6 solvents (main component: 30～60 ℃ of sherwood oils and other ethers) by method for producing casein by using leaching.

Background technology

At present, domestic casein research field or manufacturer are all with mechanical phonograph recorder separation (disk centrifuge: the principle that adopts difference in specific gravity) separate, degreasing, purifying produce casein (trade(brand)name: casein food grade), the general lipid content of the casein that mechanical phonograph recorder separation is produced is between 2.0～2.5%, owing to be subjected to the restriction of fatty high factor in the raw material, the lipid content in the casein product is difficult to by mechanical phonograph recorder separation it be dropped to below 1.0%.The lipid content height directly has influence on casein series product quality grade.Its specific embodiment is: and thick casein (song draws) → pulverizing → dissolving (Gu: liquid=1: 10)+10%NaOH solution adjust pH 9～11, temperature: 50～65 ℃ → filtration → disk centrifuge degreasing → acidifying (15%HCL solution adjust pH 4.6) → dehydration → granulation → drying → product → test package.Such production technique is owing to lipid content height in the raw material is different, and the product lipid content of producing also height is different, causes product to be lacked competitiveness on market.

Summary of the invention

The objective of the invention is to produce the deficiency of casein technology in order to solve above-mentioned mechanical phonograph recorder separation, provide mixture solvent or 30～60 ℃ of sherwood oils of a kind of grease liquefied butane that manufacture field adopts and propane to get except that fat residual in the casein with other ether solvent lixiviation process, thereby solve thoroughly that the casein series product are subjected in the raw material that the lipid content height is different, the mechanical phonograph recorder separation restriction of production causes in the casein series product lipid content height inconsistent, and a kind of method of method for producing casein by using leaching is provided

Technical scheme of the present invention is: the method for method for producing casein by using leaching, it is characterized in that adopting the mixture solvent of liquefied butane and propane or 30～60 ℃ of sherwood oils to get except that production method fatty in the casein with other ether solvent lixiviate, be raw material mainly with thick casein (song draws), get a certain amount of thick casein (song draws) and add No. 4 solvents of 6～10 times or No. 6 solvents at normal temperature and certain pressure (under 0.3～0.8MPa), reverse-flow with subcritical fluids, or solvent is reclaimed in the fat back that utilizes the soxhlet extraction principle to leach in the thick casein, add a certain amount of water in the thick casein that removes fat with getting, add 10%NaOH solution adjust pH 9～11 then, heating exists temperature: between 50～65 ℃ it is dissolved fully, separate acidifying by the ash melting type separating machine, dehydration, granulation, thereby dry back obtains the casein product of lipid content≤0.3%.

The method of described method for producing casein by using leaching is characterized in that the preparation process of this method is as follows:

(a), dissolving

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, mixture solvent or 30～60 ℃ of sherwood oils and other ether solvent of adding 6～10 parts of liquefied butanes and propane then, at normal temperature and certain pressure (0.3～0.8MPa), or under 30～60 ℃, reverse-flow with subcritical fluids, or utilize the soxhlet extraction principle to leach fat 45～60min, reclaim solvent, to get the water that adds 10～15 parts in the thick casein that removes fat then, 50～65 ℃ of warmings while stirring, add 1～5 part of 10～50%NaOH solution adjust pH 9～11 again and continue to stir 30～50min, it is dissolved fully, prepare to filter.

(b), filter

The casein solution that the dissolving of (a) step is good is standby with 80～120 order nylon net filters, reclaims residual assorted;

(c), separate

Above-mentioned filtered liquid gradation is joined in the centrifuge tube, under 3000～6000r/min, carry out centrifugation 10～15min, stop centrifugal taking-up centrifuge tube, topple over and the containers for future use that supernatant liquor merges to certain volume, reclaim throw out;

(d), acidifying

The solution that above-mentioned centrifugation is good is preheating between 38～50 ℃, and the hydrochloric acid that adds 1～3 part of 4～12mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 10～15min;

(e), clean

Filter the acidic solution in the above-mentioned acidifying albumen, add the hot water between 38～50 ℃ of the equal-volumes, soak 10～15min, prepare to filter;

(f), filter

With 80～120 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55～60%, prepares granulation with above-mentioned cleaned albumen and scavenging solution;

(h), granulation, drying

Water ratio 55～60% caseins that above-mentioned filtration is good are crossed 30 order sub-sieves, make wet casein order count maximum and are no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

Advantage of the present invention and effect:

Product index:

1, physical and chemical index:

Sense organ: milky white or faint yellow fine granularity or powder;

Smell: no special odor;

Nitrogen content: 〉=14.5%

Moisture :≤12.0%

Ash content :≤2.0%

PH value: 5.5～6.0

Fat :≤0.3%

2, microbiological indicator:

Total plate count≤30cfu/g

Coliform MPN/100g≤40

Pathogenic bacterium must not detect

3, heavy metal index:

Arsenic (in As)≤0.0002%

Plumbous (in Pb)≤0.002%.

The invention solves the high problem of lipid content in the mechanical phonograph recorder separation production casein product, this arts demand is employed leaching plant in oil prodution industry, on the basis of original casein production technique, increase step leaching step, lipid content in the casein product can be reduced to below 0.3%, quality product is better than the product that traditional technology is produced.

Description of drawings

Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.

Accompanying drawing is technological process of production figure of the present invention.

Embodiment

Embodiment 1:

1, dissolving

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, the mixture solvent that adds 6 parts of liquefied butanes and propane then, at normal temperature and certain pressure (0.3～0.8MPa), with the fatty 45min of the reverse-flow leaching of subcritical fluids, reclaim solvent, will get the water that adds 10 parts in the thick casein that removes fat then, 50 ℃ of warmings while stirring, add 1 part of 50%NaOH solution adjust pH 11.0 again and continue to stir 30min, it is dissolved fully, prepare to filter.

2, filter

The casein solution that the 1st one-step hydrolysis is good reclaims residual assorted with 80 order nylon net filters.

3, centrifugation

The casein solution gradation that above-mentioned filtration is good joins in the centrifuge tube, carries out centrifugal 15min under 3600r/min, stops centrifugal taking-up centrifuge tube, topples over the containers for future use that supernatant liquor merges to certain volume, reclaims throw out.

4, acidifying

The solution that above-mentioned centrifugation is good is preheating to 38 ℃, and the hydrochloric acid that adds 1 part of 12mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 10min.

5, clean

Filter the acidic solution in the above-mentioned acidizing fluid, add the hot water of 38 ℃ of equal-volumes, soak 15min, prepare to filter.

6, filter

With 80 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55%, prepares granulation with above-mentioned cleaned albumen and scavenging solution.

7, granulation, drying

Water ratio 55% casein that above-mentioned filtration is good is crossed 30 order sub-sieves, makes wet casein order count maximum and is no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

Example 2

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, the mixture solvent that adds 10 parts of liquefied butanes and propane then, at normal temperature and certain pressure (0.3～0.8MPa), with the fatty 45min of the reverse-flow leaching of subcritical fluids, reclaim solvent, will get the water that adds 15 parts in the thick casein that removes fat then, 56 ℃ of warmings while stirring, add 5 parts of 10%NaOH solution adjust pHs 9.0 again and continue to stir 50min, it is dissolved fully, prepare to filter.

2, filter

The casein solution that the 1st one-step hydrolysis is good reclaims residual assorted with 120 order nylon net filters.

3, centrifugation

The casein solution gradation that above-mentioned filtration is good joins in the centrifuge tube, carries out centrifugal 10min under 6000r/min, stops centrifugal taking-up centrifuge tube, topples over the containers for future use that supernatant liquor merges to certain volume, reclaims throw out.

4, acidifying

The solution that above-mentioned centrifugation is good is preheating to 38 ℃, and the hydrochloric acid that adds 3 parts of 4mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 15min.

5, clean

Filter the acidic solution in the above-mentioned acidizing fluid, add the hot water of 50 ℃ of equal-volumes, soak 10min, prepare to filter.

6, filter

With 120 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55%, prepares granulation with above-mentioned cleaned albumen and scavenging solution.

7, granulation, drying

Water ratio 60% casein that above-mentioned filtration is good is crossed 30 order sub-sieves, makes wet casein order count maximum and is no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

Example 3

1, dissolving

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, add 6 parts of 30～60 ℃ of sherwood oils and other ether solvent then, under 30 ℃ of temperature, leach fatty 60min with the soxhlet extraction principle, reclaim solvent, will get the water that adds 10 parts in the thick casein that removes fat then, warming while stirring to 50 ℃, add 1 part of 50%NaOH solution adjust pH 11.0 again and continue to stir 30min, it is dissolved fully, prepare to filter.

2, filter

The casein solution that the 1st one-step hydrolysis is good reclaims residual assorted with 80 order nylon net filters.

3, centrifugation

The casein solution gradation that above-mentioned filtration is good joins in the centrifuge tube, carries out centrifugal 15min under 3600r/min, stops centrifugal taking-up centrifuge tube, topples over the containers for future use that supernatant liquor merges to certain volume, reclaims throw out.

4, acidifying

The solution that above-mentioned centrifugation is good is preheating to 38 ℃, and the hydrochloric acid that adds 1 part of 12mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 10min.

5, clean

Filter the acidic solution in the above-mentioned acidizing fluid, add the hot water of 38 ℃ of equal-volumes, soak 15min, prepare to filter.

6, filter

With 80 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55%, prepares granulation with above-mentioned cleaned albumen and scavenging solution.

7, granulation, drying

Water ratio 55% casein that above-mentioned filtration is good is crossed 30 order sub-sieves, makes wet casein order count maximum and is no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

Example 4

1, dissolving

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, add 10 parts of 30～60 ℃ of sherwood oils and other ether solvent then, under 60 ℃ of temperature, leach fatty 60min with the soxhlet extraction principle, reclaim solvent, will get the water that adds 15 parts in the thick casein that removes fat then, warming while stirring to 56 ℃, add 5 parts of 10%NaOH solution adjust pHs 9.0 again and continue to stir 50min, it is dissolved fully, prepare to filter.

2, filter

The casein solution that the 1st one-step hydrolysis is good reclaims residual assorted with 120 order nylon net filters.

3, centrifugation

The casein solution gradation that above-mentioned filtration is good joins in the centrifuge tube, carries out centrifugal 10min under 6000r/min, stops centrifugal taking-up centrifuge tube, topples over the containers for future use that supernatant liquor merges to certain volume, reclaims throw out.

4, acidifying

The solution that above-mentioned centrifugation is good is preheating to 38 ℃, and the hydrochloric acid that adds 3 parts of 4mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 15min.

5, clean

Filter the acidic solution in the above-mentioned acidizing fluid, add the hot water of 50 ℃ of equal-volumes, soak 10min, prepare to filter.

6, filter

With 120 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55%, prepares granulation with above-mentioned cleaned albumen and scavenging solution.

7, granulation, drying

Water ratio 60% casein that above-mentioned filtration is good is crossed 30 order sub-sieves, makes wet casein order count maximum and is no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

Claims (2)

1. the method for a method for producing casein by using leaching, it is characterized in that: adopt the mixture solvent of liquefied butane and propane or 30～60 ℃ of sherwood oils to get except that production method fatty in the casein with other ether solvent lixiviate, be raw material mainly with thick casein (song draws), get a certain amount of thick casein (song draws) and add the mixture solvent of 6～10 times liquefied butane and propane or 30～60 ℃ of sherwood oils and other ether solvent at normal temperature and certain pressure (under 0.3～0.8MPa), reverse-flow with subcritical fluids, or solvent is reclaimed in the fat back that utilizes the soxhlet extraction principle to leach in the thick casein, add a certain amount of water in the thick casein that removes fat with getting, add 10%NaOH solution adjust pH 9～11 then, heating exists temperature: between 50～65 ℃ it is dissolved fully, separate acidifying by the ash melting type separating machine, dehydration, granulation, thereby dry back obtains the casein product of lipid content≤0.3%.

2. the method for method for producing casein by using leaching according to claim 1 is characterized in that the preparation process of this method is as follows:

(a), dissolving

Accurately taking by weighing 1 part of thick casein (song draws) joins in the batch extractor of certain volume, mixture solvent or 30～60 ℃ of sherwood oils and other ether solvent of adding 6～10 parts of liquefied butanes and propane then, at normal temperature and certain pressure (0.3～0.8MPa), or under 30～60 ℃, reverse-flow with subcritical fluids, or utilize the soxhlet extraction principle to leach fat 45～60min, reclaim solvent, to get the water that adds 10～15 parts in the thick casein that removes fat then, 50～65 ℃ of warmings while stirring, add 1～5 part of 10～50%NaOH solution adjust pH 9～11 again and continue to stir 30～50min, it is dissolved fully, prepare to filter;

(b), filter

The casein solution that the dissolving of (a) step is good is standby with 80～120 order nylon net filters, reclaims residual assorted;

(c), separate

Above-mentioned filtered liquid gradation is joined in the centrifuge tube, under 3000～6000r/min, carry out centrifugation 10～15min, stop centrifugal taking-up centrifuge tube, topple over and the containers for future use that supernatant liquor merges to certain volume, reclaim throw out;

(d), acidifying

The solution that above-mentioned centrifugation is good is preheating between 38～50 ℃, and the hydrochloric acid that adds 1～3 part of 4～12mol/L stirs acidifying, and adjust pH to casein iso-electric point 4.6 is a terminal point, leaves standstill 10～15min;

(e), clean

Filter the acidic solution in the above-mentioned acidifying albumen, add the hot water between 38～50 ℃ of the equal-volumes, soak 10～15min, prepare to filter;

(f), filter

With 80～120 order nylon net filter mistakes, extruding makes the moisture content in the albumen drop to 55～60%, prepares granulation with above-mentioned cleaned albumen and scavenging solution;

(h), granulation, drying

Water ratio 55～60% caseins that above-mentioned filtration is good are crossed 30 order sub-sieves, make wet casein order count maximum and are no more than 30 orders; Be placed on drying in the blowing-type loft drier then, the finished product water ratio is no more than 12%.

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