CN101717440B - method for preparing casein - Google Patents
method for preparing casein Download PDFInfo
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- CN101717440B CN101717440B CN2009102289975A CN200910228997A CN101717440B CN 101717440 B CN101717440 B CN 101717440B CN 2009102289975 A CN2009102289975 A CN 2009102289975A CN 200910228997 A CN200910228997 A CN 200910228997A CN 101717440 B CN101717440 B CN 101717440B
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Abstract
The invention relates to a method for preparing casein. The method comprises the following steps of: preparing reconstituted milk by taking substandard milk powder, crude casein, liquid milk, and the like as main raw materials, precipitating the casein by utilizing the characteristic that the isoelectric pointof the casein is 4.6 and utilizing dilute hydrochloric acid as a coagulator to be directly used for the precipitation process of the casein, breaking the structure of lipid-protein compound in the milk powder by utilizing an ammonia solution, dissociating combined fattiness, extracting the fattiness by utilizing ethyl ether and petroleum ether, separating an organic layer, agglomerating the casein again by utilizing the dilute hydrochloric acid again, washing and dehydrating the casein to obtain half-wet casein blocks, and drying granulated casein in a two-section mode to obtain finished casein products. The invention greatly enlarges the types of raw materials for preparing the casein, can utilize the substandard milk powder, the crude casein, fresh milk with excessive acidity and fresh milk containing antibiotics to be not suitable for processing and utilization, and has the advantages of simple production process, low cost, high product purity, complete utilization of resources, recycled solved, safe production process and easy control of quality.
Description
Technical field
The invention belongs to dairy technology and light industry industry field, relate in particular to a kind of with the excessive fresh milk of defective milk powder, rough casein food grade, acidity, contain the method that antibiotic fresh milk is the feedstock production casein food grade.
Background technology
Casein food grade is widely used in aspects such as food, coating, tamanori, medicine, plastic-substitute, precise electronic, is a kind of food and light industry industry multipurpose additive.The particulate state or the pulverulent material of casein food grade casein containing protein more than 92%, the little Huang of color and luster or oyster white, no stink are widely used in the synthetic galalith of industry, casein glue production, sizing agent processing etc.Cheese have following characteristics and character: be prone to the suction conglomeration and expand; The casein macromole makes solution produce higher viscosity, and retrogradation is thick, becomes gel again after the solution cooling, becomes solution after gel is heated again.The gel high resilience, and can keep moisture, dehydration is not shunk hardly; Have very strong emulsification thickening power, its molecule has many hydrophilic radicals and hydrophobic group, and adsorbable water and lipoid material make solution have greasy characteristic after the emulsification; The hydrochloric acid casein molecular energy is isolated micro-bubble, and keeps the foam nonjoinder, and is not broken.Hydrochloric acid casein has a wide range of applications in industries such as leather, light textile, papermaking, national defense industry as a kind of important chemical material.Aspect papermaking, as sizing agent, lustering agent, tamanori etc.; In leather industry, be used for artificial leather tanning agent, tamanori etc.; In building trade, be a kind of waterproof, anti-electricity, HS, decorative coating; In the steel equipment manufacturing and in using as high firmness acid-proof coating; Aspect electrochemistry, be used for electroplating industry wastewater treatment and non-ferrous metal and reclaim; On non-metallic material such as pottery, glass, carry out the surface treatment of the electroless plating of metallic substance such as copper, nickel, cobalt; Also be the raw material of producing the casein food grade plastics, be used to produce senior artwork such as ivory substitute, key, chess piece, beads, necklace, billiard ball and senior button etc., inside and outside market, native land is bigger to the demand of casein food grade, and development prospect is wide.
At present the casein food grade produced of countries in the world is to be raw material with bright skimming milk (about lipid content 0.05%); With acid or ferment rennet cohesion casein; The product of processing through dehydrating, its staple is a casein, needs a large amount of high quality raw material cow's milk in the manufacturing processed.Because casein food grade is comparatively harsh to ingredient requirement, and China's fresh milk supply falls short of demand, so seldom produce casein food grade with this method.The method of China's traditional mode of production casein food grade is to be the feedstock production casein food grade with " song draws ", but the herdsman because the production environment sanitary condition is poor, makes " song draws " oxidative rancidity when extensive style production " song draws "; Impurity is many, and the casein food grade kind of producing with " song draws " is single, lacks deep processed product, and processing technology falls behind; Be simply equipped, smell is not good, and purity is not enough, unstable product quality; Industrial scale is little, and level of management are low simultaneously, and economic benefit is not high.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art; Provide a kind of with the too high fresh milk of defective milk powder, rough casein food grade, acidity or contain the method that antibiotic fresh milk is the feedstock production casein food grade; Casein food grade purity through present method preparation is high, and color and luster is milky white, free from extraneous odour; Stay in grade, Application Areas is extensive.
The objective of the invention is to realize through following technical scheme:
A kind of preparation casein food grade method, step is following:
(1) dissolving: with milk products raw material mixed dissolution in mixing tank, stir, feed liquid is pumped into an acid jar;
(2) acid: concentrated hydrochloric acid and water after 1: 7~9 dilutions, are joined in the acid jar, make the pH of feed liquid reach 4.6; Casein coagulation is separated out; Keep reaction 0.5~1h, continue to add the hydrochloric acid diluent and make the pH of feed liquid reach 4.2, react 0.5~1h again; Remove waste liquid, obtain the casein throw out;
(3) mild alkaline treatment: the casein throw out is changed in the retort, be incorporated as the water of 1~3 times of casein throw out total amount, mixing; And then add the ammoniacal liquor of 1~3 times of casein amount, and abundant mixing, reaction 0.5~1h under 55~65 ℃ of stirrings reacts postcooling to 25~30 ℃;
(4) degreasing: add the industrial alcohol of the reduction of feed volume 1/2 in the retort, fully mixing; Add the ether suitable with amount of alcohol again, stir 5~10min, add and the sherwood oil of ether equivalent again, restir 20~30min leaves standstill 8~16h, and it is to be recycled to remove the ether layer;
(5) secondary point acid: the feed liquid in the retort is pumped into an acid jar again, concentrated hydrochloric acid and water after 1: 6~9 dilutions, are joined in the feed liquid in the acid jar, make its pH reach 4.6, casein coagulation is separated out, and keeps and reacts 0.5~1h; Continue to add the pH to 4.2 that the hydrochloric acid diluent makes feed liquid, react 0.5~1h again, it is to be recycled to remove waste liquid, obtains the casein throw out;
(6) secondary washing dehydration: wash the casein throw outs 2~3 times with 20~30 ℃ of clear water, and constantly stir, make grumeleuse all loose into particulate state; After wet casein after the washing filtered with 150~350 order filter clothes, dewatering to water ratio with centrifugal drier was lower than 50%, formation casein piece;
(7) granulation: the casein piece is put into tablets press count granulation by required order;
(8) drying: with the casein that granulation finishes, the fs places the negative pressure hot air dryer, drying temperature≤45 ℃, and pressure-0.3~-0.5KPa, time 10~20min, the powder moisture content can reduce to 25~40%; Subordinate phase places the continuous-type microwave drying bed, frequency 2500MHz, and 40 ℃ of drying temperatures, the powder moisture content is reduced to below 6%, and casein food grade gets product.
And said milk products comprise the excessive fresh milk of defective milk powder, rough casein food grade, acidity, contain antibiotic fresh milk.
And, milk products raw material and clean water by weight 1: 6~9 in mixing tank mixed dissolution, the temperature of this clean water is 30~50 ℃.
Advantage of the present invention and positively effect are:
1, among the present invention; Adopt strong aqua to break the structure of the lipid-protein complex in the dairy products; To pass through in the milk powder of homogenization treatment and separate with the fat of protein bound; The mixing fluid power of ether and sherwood oil is come out the extracting fat in Ruzhong smoothly, make the plain purpose of low fat cheese thereby reach.
2, use industrial alcohol to quicken caseic sedimentation, play inorganic and the well-defined effect of ether layer of making, ethanol also can dissolve the phospholipid substance in the feed liquid simultaneously, makes casein be able to purifying.
3, raw material of the present invention can be the excessive fresh milk of defective milk powder, rough casein food grade, acidity or contain antibiotic fresh milk etc.; Particularly can use whole milk powder to prepare casein food grade; Broken through the technology of the homogeneous milk powder degreasing of high fat content, be of great importance.The raw material type for preparing casein food grade has been expanded in the realization of this invention greatly, is confined to the of inferior quality yak of fresh milk and quality " song draws " no longer singlely; Simultaneously, but the rotten skim-milk and whole milk powder equal utilization of waste material of inferior quality with quality are prepared into the high casein food grade product of valency of fine quality, have significantly reduced wastage of material, have reduced the loss of enterprise, have promoted economic benefit of enterprises.Say that from technological angle production technique is simple, process is easy to control, less demanding to equipment; Use therein organic solvent can reclaim, and uses repeatedly, has reduced production cost; Say that from the product angle made casein food grade is satisfied with the demand industry of all kinds of casein food grade, product gas purity and quality have all reached gold standard: yield rate 21%; Oyster white, free from extraneous odour, protein>=93%; Fat≤0.15%, ash content≤2.4%, moisture≤6%; Cl ions≤0.004%, acidity≤35 ° T.
Embodiment
Below in conjunction with embodiment, the present invention is further specified, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1:
A kind of preparation casein food grade method, step is:
(1) dissolving: the 6t whole milk powder is placed dissolving vessel, add the 44t clean water, be heated to 40 ℃, stir;
(2) acid: feed liquid is pumped into an acid jar, slowly add Hydrogen chloride (concentrated hydrochloric acid: water=1: 8), make its pH reach 4.6 (measuring) with pH meter; Casein coagulation is separated out, and keeps reaction 1h, continues to add acid and reaches 4.2 to pH; Make its reaction 30min again, remove waste liquid, obtain the casein throw out;
(3) mild alkaline treatment: the casein throw out is changed in the retort, add 3t water, mixing adds 2t ammoniacal liquor, abundant mixing, and reaction 30min under 65 ℃ of stirrings reacts postcooling to 25 ℃;
(4) degreasing: add the 2t absolute ethyl alcohol, fully mixing adds the 2t ether, stirs 10min, adds the 2t sherwood oil, and restir 30min leaves standstill 10h, and it is to be recycled to remove the ether layer;
(5) secondary point acid: feed liquid is pumped into an acid jar, slowly add Hydrogen chloride (concentrated hydrochloric acid: water=1: 8), make its pH reach 4.6 (measuring) with the pH test paper; Casein coagulation is separated out; Keep reaction 1h, continue to add acid, make its reaction 30min again to pH to 4.2; It is to be recycled to remove waste liquid, obtains the casein throw out;
(6) secondary washing dehydration: wash caseins 3 times with 30 ℃ of clear water, and constantly stir, make grumeleuse all loose into particulate state; With after the 150 order filter clothes filtrations, dewatering to water ratio with centrifugal drier is lower than 50% with the wet casein after the washing;
(7) granulation: the casein piece is put into tablets press count granulation by required order;
(8) drying: with the casein that granulation finishes, the fs places the negative pressure hot air dryer, drying temperature≤45 ℃, and pressure-0.3~-0.5KPa, time 10~12min, the powder moisture content can reduce to 25~40%; Subordinate phase places the continuous-type microwave drying bed, frequency 2500MHz, and 40 ℃ of drying temperatures, the powder moisture content is reduced to below 6%, and casein food grade gets product.
Its product quality indicator is: yield rate 21%, oyster white, free from extraneous odour, protein>=93%, fat≤0.15%, ash content≤2.4%, moisture≤6%, cl ions≤0.004%, acidity≤35 ° T.
Embodiment 2:
(1) dissolving: the thick casein food grade pulverizing of 2t is placed in the dissolving vessel, adds the dissolving of 3t clean water;
(2) acid:, therefore needn't carry out a sour work step again because present embodiment is that the thick casein food grade of employing is a raw material;
(3) mild alkaline treatment: add 3.5t ammoniacal liquor again, abundant mixing, reaction 30min under 65 ℃ of stirrings reacts postcooling to 25 ℃;
(4) degreasing: add the 3.5t industrial alcohol, fully mixing adds the 3.5t ether, stirs 10min, adds the 3.5t sherwood oil, and restir 30min leaves standstill 10h, and it is to be recycled to remove the ether layer;
(5) secondary point acid: feed liquid is pumped into an acid jar, slowly add Hydrogen chloride (concentrated hydrochloric acid: water=1: 8), make its pH reach 4.6 (measuring) with the pH test paper; Casein coagulation is separated out; Keep reaction 1h, continue to add acid, make its reaction 30min again to pH to 4.2; It is to be recycled to remove waste liquid, obtains the casein throw out;
(6) secondary washing dehydration: wash caseins 3 times with 30 ℃ of clear water, and constantly stir, make grumeleuse all loose into particulate state; With after the 150 order filter clothes filtrations, dewatering to water ratio with centrifugal drier is lower than 50% with the wet casein after the washing;
(7) granulation: the casein piece is put into tablets press count granulation by required order;
(8) drying: with the casein that granulation finishes, the fs places the negative pressure hot air dryer, drying temperature≤45 ℃, and pressure-0.3~-0.5KPa, time 10~12min, the powder moisture content can reduce to 25~40%; Subordinate phase places the continuous-type microwave drying bed, frequency 2500MHz, and 40 ℃ of drying temperatures, the powder moisture content is reduced to below 6%, and casein food grade gets product.
Product quality indicator is: yield rate 78%, oyster white, free from extraneous odour, protein>=93%, fat≤0.15%, ash content≤2.2%, moisture≤6%, cl ions≤0.004%, acidity≤35 ° T.
Embodiment 3:
(1) dissolving: the yogurt of 30t fermentation failure is placed dissolving vessel, be heated to 70 ℃, stir 3min, milk-acid bacteria is lost activity;
(2) acid: feed liquid is pumped into an acid jar, slowly add Hydrogen chloride (concentrated hydrochloric acid: water=1: 9), make its pH reach 4.6 (measuring) with pH meter; Casein coagulation is separated out, and keeps reaction 1h, continues to add acid and reaches 4.2 to pH; Make its reaction 30min again, remove waste liquid, obtain the casein throw out;
(3) mild alkaline treatment: the casein throw out is changed in the retort, add 1.5t water, mixing adds 1.5t ammoniacal liquor, abundant mixing, and reaction 30min under 65 ℃ of stirrings reacts postcooling to 25 ℃;
(4) degreasing: add the 1.5t industrial alcohol, fully mixing adds the 1.5t ether, stirs 10min, adds the 1.5t sherwood oil, and restir 30min leaves standstill 10h, and it is to be recycled to remove the ether layer;
(5) secondary point acid: feed liquid is pumped into an acid jar, slowly add Hydrogen chloride (concentrated hydrochloric acid: water=1: 9), make its pH reach 4.6 (measuring) with the pH test paper; Casein coagulation is separated out; Keep reaction 1h, continue to add acid, make its reaction 30min again to pH to 4.2; It is to be recycled to remove waste liquid, obtains the casein throw out;
(6) secondary washing dehydration: wash caseins 3 times with 30 ℃ of clear water, and constantly stir, make grumeleuse all loose into particulate state; With after the 150 order filter clothes filtrations, dewatering to water ratio with centrifugal drier is lower than 50% with the wet casein after the washing;
(7) granulation: the casein piece is put into tablets press count granulation by required order;
(8) drying: with the casein that granulation finishes, the fs places the negative pressure hot air dryer, drying temperature≤45 ℃, and pressure-0.3~-0.5KPa, time 10~12min, the powder moisture content can reduce to 25~40%; Subordinate phase places the continuous-type microwave drying bed, frequency 2500MHz, and 40 ℃ of drying temperatures, the powder moisture content is reduced to below 6%, and casein food grade gets product.
Product quality indicator is: yield rate 2.4%, oyster white, free from extraneous odour, protein>=92%, fat≤0.15%, ash content≤2.2%, moisture≤6%, cl ions≤0.004%, acidity≤50 ° T.
Principle of the present invention is:
Utilize ammoniacal liquor to break the structure of the lipid-protein complex in the milk powder, i.e. the present invention uses weak base-WITH AMMONIA TREATMENT, in emulsion, adds ammoniacal liquor; The pH value is away from the iso-electric point of casein protein; Thereby make attached to the dissolving of the casein on the Oil globule, expose inner fat, then; With ether, sherwood oil extraction agent, thereby realize separating of butterfat and non-fat composition as fat; Add ethanol; As dewatering agent; It can make from fatty spheroid dissolve the casein sex change of getting off solidify and be deposited in inorganic mutually, and make inorganic and organic phase layering clear, simultaneously dissolve with ethanol thing such as phospholipid substance are dissolved in wherein; Add sherwood oil and can prevent that ether by water saturation, is beneficial to the process operation in later stage.
Claims (3)
1. one kind prepares the casein food grade method, and it is characterized in that: step is following:
(1) dissolving: with milk products raw material mixed dissolution in mixing tank, stir, feed liquid is pumped into an acid jar;
(2) acid: concentrated hydrochloric acid and water after 1: 7~9 dilutions, are joined in the acid jar, make the pH to 4.6 of feed liquid; Casein coagulation is separated out; Keep reaction 0.5~1h, continue to add the hydrochloric acid diluent and make the pH of feed liquid reach 4.2, react 0.5~1h again; Remove waste liquid, obtain the casein throw out;
(3) mild alkaline treatment: the casein throw out is changed in the retort, be incorporated as the water of 1~3 times of casein throw out total amount, mixing; And then be incorporated as the ammoniacal liquor of 1~3 times of casein throw out total amount, and abundant mixing, reaction 0.5~1h under 55~65 ℃ of stirrings reacts postcooling to 25~30 ℃;
(4) degreasing: add the industrial alcohol of the reduction of feed volume 1/2 in the retort, fully mixing; Add the ether suitable with amount of alcohol again, stir 5~10min, add and the sherwood oil of ether equivalent again, restir 20~30min leaves standstill 8~16h, and it is to be recycled to remove the ether layer;
(5) secondary point acid: the feed liquid in the retort is pumped into an acid jar again, concentrated hydrochloric acid and water after 1: 6~9 dilutions, are joined in the feed liquid in the acid jar, make its pH reach 4.6, casein coagulation is separated out, and keeps and reacts 0.5~1h; Continue to add the pH to 4.2 that the hydrochloric acid diluent makes feed liquid, react 0.5~1h again, it is to be recycled to remove waste liquid, obtains the casein throw out;
(6) secondary washing dehydration: wash the casein throw outs 2~3 times with 20~30 ℃ of clear water, and constantly stir, make grumeleuse all loose into particulate state; After wet casein after the washing filtered with 150~350 order filter clothes, dewatering to water ratio with centrifugal drier was lower than 50%, formation casein piece;
(7) granulation: the casein piece is put into tablets press count granulation by required order;
(8) drying: with the casein that granulation finishes, the fs places the negative pressure hot air dryer, drying temperature≤45 ℃, and pressure-0.3~-0.5KPa, time 10~20min, the powder moisture content can reduce to 25~40%; Subordinate phase places the continuous-type microwave drying bed, frequency 2500MHz, and 40 ℃ of drying temperatures, the powder moisture content is reduced to below 6%, and casein food grade gets product.
2. preparation casein food grade method according to claim 1 is characterized in that: said milk products comprise the excessive fresh milk of defective milk powder, rough casein food grade, acidity, contain antibiotic fresh milk.
3. preparation casein food grade method according to claim 1 is characterized in that: said milk products raw material and clean water by weight 1: 6~9 in mixing tank mixed dissolution, the temperature of this clean water is 30~50 ℃.
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Families Citing this family (7)
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CN102165988A (en) * | 2011-03-14 | 2011-08-31 | 天津科技大学 | Method for preparing rennet casein by using cow's milk |
CN105315358A (en) * | 2015-11-06 | 2016-02-10 | 甘肃普罗生物科技有限公司 | Method for producing casein through dry sterilization |
CN108567045B (en) * | 2017-03-14 | 2021-03-26 | 中国农业大学 | Method for gradient pH value-grading production of casein by taking Triton as raw material |
CN108586598A (en) * | 2018-04-18 | 2018-09-28 | 阿坝县凯安生物制品有限公司 | A kind of production method with the wet cheese processing fresh milk grade casein of yak |
CN111053147A (en) * | 2019-12-13 | 2020-04-24 | 四川省都江堰市岷安生物制品有限责任公司 | Process for producing high-protein zero-fat casein from yak fresh milk |
CN111011534A (en) * | 2019-12-25 | 2020-04-17 | 西南民族大学 | Method for improving color of yak Qula casein |
CN115989846B (en) * | 2023-03-21 | 2023-05-30 | 中国农业大学 | Graded preparation method of trovain |
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CN1587336A (en) * | 2004-07-13 | 2005-03-02 | 甘肃省商业科技研究所 | Dry powder casein glue and its producing process |
CN1692785A (en) * | 2005-06-23 | 2005-11-09 | 甘肃农业大学 | Art for prodn. of lactic acid casein using |
CN101085807A (en) * | 2006-09-01 | 2007-12-12 | 甘肃华羚生物技术研究中心 | Method for preparing high viscosity hydrochloric acid casein |
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CN1587336A (en) * | 2004-07-13 | 2005-03-02 | 甘肃省商业科技研究所 | Dry powder casein glue and its producing process |
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