CN102773140A - Manufacturing method for ultrafine shell powder - Google Patents

Manufacturing method for ultrafine shell powder Download PDF

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Publication number
CN102773140A
CN102773140A CN2011101182183A CN201110118218A CN102773140A CN 102773140 A CN102773140 A CN 102773140A CN 2011101182183 A CN2011101182183 A CN 2011101182183A CN 201110118218 A CN201110118218 A CN 201110118218A CN 102773140 A CN102773140 A CN 102773140A
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shell
powder
raw material
cleaning
particle diameter
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王志平
于晶辉
李清德
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Abstract

The invention discloses a manufacturing method for ultrafine shell powder. The manufacturing method is realized through the following seven processing steps: cleaning, drying, primary crushing, crushing of fine powder, crushing of micro powder, processing of nanometer powder and post processing. According to the invention, conch shells which are a byproduct obtained after meat of conches is removed through aquatic product processing are used as a raw material; process flow of the manufacturing method is simple, different finished products can be obtained at different stages, each processing step is carried out at a low temperature, physical processing is employed, and therefore, biological activity of the shell powder is maintained and loss and denaturation of a majority of active substances are avoided.

Description

The manufacturing approach of shell ultra micro powder
Technical field
The present invention relates to a kind of manufacturing approach of shell ultra micro powder, a kind of specifically base substance structures such as oyster shell, Xiayi shellfish shell, scallop shell, mussel shell, conch shell of utilizing are the marine organisms hard shell of the calcium carbonate method for raw material production shell ultra micro powder.
Background technology
As everyone knows, in field of powder engineering, powder granule can be divided into five types of coarse dispersions, middle fine powder body, fine powder body, powder body, nano-powder.The powder of particle diameter ﹥ 0.5mm is called coarse dispersion, can be made by Mechanical Crushing; Fine powder body during the powder of particle diameter between 0.074~0.5mm is called can be made by the machinery corase grind; Particle diameter is called the fine powder body at the powder of 10~74 μ m, can be made by mechanical fine grinding; The powder of particle diameter between 0.1~10 μ m is called powder body, and powder body is claimed superfine powder again in some data, can be made by ultra-fine mill of machinery or chemical method; The powder of particle diameter ﹤ 100nm is a nano-powder, is generally made by chemical method.
The said ultra micro powder of this patent comprises powder body and nano-powder.
There is data to show, contains trace elements such as several amino acids, calcium, protein, crude fat and manganese, zinc, iron, potassium, magnesium phosphorus in the shell.Wherein, calcium carbonate 90-95%, protein 0.48%, crude fat 0.134%, moisture < 0.04%; In the per kilogram shell, contain manganese 81.0mg, zinc 2.90mg, iron 285mg, potassium 214mg, magnesium 2.04 * 1000mg, phosphorus 48.0mg.The powder that utilizes shell to produce is widely used in fields such as food, livestock and poultry, industrial art, plastics and chemical industry, and highly purified oyster shell whiting can be used as pharmaceutical calcium, the food raw material with calcium.
Make animal and fowl fodder calcium source additive with oyster shell whiting, can promote the livestock and poultry bone growth, increase the output of egg, milk and improve its quality, improve the livestock and poultry resistance against diseases simultaneously and strengthen its digestive function.In the chicken feed, add oyster shell whiting and can obviously improve eggshell quality, improve laying rate; In pig feed, add 1% oyster shell whiting, can satisfy pig grow necessary calcium, phosphorus and other trace element.
Oyster shell whiting also can be used as environment-friendly fertilizer, in and acid ground, loose improving the soil improved the taste of crops.
The processing method of existing oyster shell whiting is difficult to reach ultra micro powder yardstick.
Summary of the invention
The objective of the invention is to provide that a kind of to adopt the shell leftover bits and pieces of processing of aquatic products be raw material, the manufacturing approach of the shell ultra micro powder that technological process is simple, with low cost.
The objective of the invention is to realize like this, in the manufacture process of shell ultra micro powder, except that cleaning link, all adopt physical method to realize the pulverizing of powder, kept the biologically active of shell powder, avoided the loss and the sex change of most of active principles.
The manufacturing approach of this shell ultra micro powder may further comprise the steps:
1. clean:, at first will clean the raw material shell surface for raw material and the finished product that obtains to clean.Matting is the pollutant that is adsorbed on shell surface in order to remove; Comprise silt, remaining shellfish meat and bacterium and heavy metal etc.; Clean the general three phases that divides, the phase I is adopted washing, tentatively removes the adsorbates such as silt that shell surface is removed easily; And, reduce pollution to cleaning agent for next stage provides the raw material of relative cleaning; The second stage of cleaning adopts Chemical cleaning, and used cleaning agent is the sodium hydrate aqueous solution of 3%~5% concentration, is adsorbed on the casting skin of shell outer surface and remaining shellfish meat with removal; Clean the phase III and adopt washing, to remove the cleaning agent and the residual contaminants of shell surface; Above three phases all adopts the rotary drum-type cleaning equipment, and utilizing between shell collides each other, rubs removes shell surface adsorbate, pollutant.As the manufactured goods powder is had special purity requirement, need clean, wash the back at above-mentioned caustic soda and add pickling process.Pickling process adopts the hydrochloric acid of 10%~15% concentration, thoroughly to dispose the residual contaminants that is adsorbed on the shellfish surface, arranges washing to remove the shell surface cleaning fluid after the pickling again.Each stage of cleaning all can add ultrasonic cleaning technology, improves cleaning efficiency, improves cleaning performance.
2. oven dry: the shell of 1. washing through step will carry out drying to remove moisture by drying plant behind draining, want the strict bake out temperature of controlling be no more than 85 ℃ during oven dry, the too high and sex change of the active ingredient Yin Wendu that prevents shell.Drying plant can adopt band drier, the cylindrical drier of oven dry vegetables.
3. elementary pulverizing: elementary pulverizing is carried out in two steps, can adopt common disintegrating apparatus such as tooth-like pulverizer, beater grinder, gyratory crusher.The shell raw material pulverizing that at first will pass through after cleaning, the oven dry is processed the shell particle that particle diameter is 2~5mm, and shell particle that then will this 2~5mm particle diameter continues to pulverize, and the acquisition particle diameter is the shell powder of 250 μ m~841 μ m.
4. fine powder is pulverized: the 3. middle shell powder through elementary pulverizing of step is carried out further grinding and processing through impact type micro mist pulverizer, obtain the shell powder of particle diameter at 5~15 μ m.
5. micro mist is pulverized: further dwindle for making the shell powder granule; Need to adopt fluid bed supersonic airstream disintegrating apparatus that the shell powder is further processed; With step 4. in the shell powder material of particle diameter 5~15 μ m through the supersonic airstream pulverization process, obtain the powder product of particle diameter 0.5~5 μ m.
6. nanoscale powder processing: adopt the processing of planetary ball mill comminuting method; Can make powder reach nanoscale; Adopting 5. middle upper level particle diameter 0.5~5 μ m powder of step is raw material, adds pure water raw material furnishing paste is carried out ball milling, and processing back product cut size can reach 40~100nm.
7. post-processed: according to the difference at oyster shell whiting body and function place, can adopt different manner of packings, be beneficial to storage, transportation and the use of manufactured goods.As be used for food, pharmaceutical field, can adopt vacuum packaging.The nanoscale paste shell powder that adopts the planetary ball mill comminuting method to obtain can directly add in food, the medicine; Obtain dry nanoscale shell powder like needs, can adopt freeze drying equipment that the paste that contains pure water is carried out freeze drying, thereby obtain the shell dry powder of nanoscale.
By in the above technological process, can obtain varigrained shell powder in different phase.As be used for food, pharmaceutical field; For guaranteeing the purity of powder, require process cleaning, sealing, can not there be introduced contaminants to sneak into raw material inside; It is high hard, wear-resisting that the piece surface of device interior and oyster shell whiting raw material contact portion is wanted, not with raw material and cleaning agent generation chemical reaction.
Advantage of the present invention:
1, raw material adopt the leftover bits and pieces of processing of aquatic products, and are with low cost;
2, technological process is simple, adopts conventional equipment mostly, and organization of production is simple and easy to do;
3, can obtain different manufactured goods in different phase, can adjust flexibly according to market demand;
4, each process procedure all is operation under low temperature environment, and adopts the processing of physics method, has kept the biologically active of shell powder, has avoided the loss and the sex change of most of active principles.
Description of drawings
Fig. 1 is a manufacturing process flow diagram of the present invention.
The specific embodiment
Shown in accompanying drawing 1: be shell ultra micro powder flow process chart in the dashed rectangle among the figure.
Be processed as example with 100kg Xiayi shellfish shell, the present invention realizes like this:
1, cleans: at first adopt the rotary drum washer water-washing method to remove adsorbates such as the surperficial silt of removing easily of Xiayi shellfish shell (byproduct of aquatic products processing, the shell of removal shellfish meat), pasture and water.Adopt 3%~5% sodium hydrate aqueous solution of heating that it was soaked 40 minutes then, heating-up temperature is no more than 60 ℃.Adopt the rotary drum-type cleaning machine that the shell that soaks, drains through sodium hydroxide solution is carried out water at last and cleaned 10~15 minutes, further remove remaining soda bath and adsorbate.
As the manufactured goods powder is had special purity requirement; Carry out a pickling again after need cleaning, wash at above-mentioned caustic soda; The salt soak of employing 10%~15% concentration 2~3 minutes; Drain the back with the washing of rotary drum-type cleaning machine,, improve purity of raw materials thoroughly to dispose the pollutant that is adsorbed on the shellfish surface.
Each stage of cleaning also can be adopted ultrasonic waves for cleaning, to improve cleaning efficiency, improves cleaning performance.
2, oven dry: the shell through washing will carry out drying to remove moisture by drying plant behind draining, drying plant can adopt the conveyor type dryer.The control bake out temperature was dried 30 minutes at 75~85 ℃ during oven dry.After above cleaning, oven dry processing, can obtain the clean shell raw material of about 90kg.
3, elementary pulverizing: elementary pulverizing is carried out in two steps, all adopts common disintegrating apparatus, like various mechanical crushing equipments such as tooth-like pulverizer, beater grinder, gyratory crushers.At first to be raw material through the shell after cleaning, drying, pulverizing back output article granularity is 2 ~ 5mm; Shell particle with this 2~5mm continues to pulverize as raw material then, and can obtain output article particle diameter is the shell powder of 250 μ m~841 μ m.The shell powder that this stage obtains can directly be used for the additive of animal and fowl fodder.
4, as seeking out more tiny powder as food, pharmaceuticals industry additive; The particle diameter in last stage of reply is that 2~5mm shell particle arranges a hydrochloric acid to clean again, and concentration of hydrochloric acid is 5%~10%, and soak time is 1 minute; Drain then, arrange washing, baking operation again; Isolate residual impurity through cyclopneumatic separator at last, obtain clean more oyster shell whiting raw material, and then it is carried out following process.Like required powder is not to be used for food, pharmaceuticals industry, then can not arrange pickling, washing, oven dry and the separation circuit in this stage.
5, fine powder is pulverized: the shell powder with through elementary pulverizing is a raw material, adopts impact type micro mist pulverizer further to process, and can obtain particle diameter is the shell powder of 5~15 μ m.
6, micro mist is pulverized: adopting fluid bed supersonic airstream disintegrating apparatus is that the upper level shell powder of 5~15 μ m is further processed to particle diameter, and product cut size can reach 0.5~5 μ m.
7, nanoscale powder processing: adopt the processing of planetary ball mill comminuting method, can make powder reach nanoscale.Adopting upper level 0.5~5 μ m powder is raw material; The ratio that adds 2.5~3 kilograms of pure water in the per kilogram raw material adds the paste that accounts for ball grinder volume 1/3rd with its furnishing paste in ball grinder, add abrading-ball then; The two total capacity can not surpass 2/3rds of ball grinder capacity; Ball milling 3 hours, can obtain particle diameter is 40~100nm paste manufactured goods, contains certain pure water.
8, post-processed: this paste manufactured goods can directly use in some occasion, also can carry out processed to it through Freeze Drying Technique, obtain the shell nano-powder.
The shell powder that is used for food, medicine should be vacuum-packed.
By in the above technological process, can obtain the shell powder of variable grain degree in different phase.For guaranteeing the purity of powder, require process cleaning, sealing, can not there be introduced contaminants to sneak into raw material inside.It is high hard, wear-resisting that the piece surface of device interior and oyster shell whiting raw material contact portion is wanted, not with processed raw material generation chemical reaction.

Claims (7)

1. the manufacturing approach of a shell ultra micro powder, it is characterized in that: this method may further comprise the steps:
1. clean: the raw material shell surface is cleaned, clean and divide three phases, the phase I is adopted washing, tentatively removes the adsorption of sediment thing that shell surface is removed easily, and for next stage provides the raw material of relative cleaning, minimizing is to the pollution of cleaning agent; The second stage of cleaning adopts Chemical cleaning, and used cleaning agent is the sodium hydrate aqueous solution of 3%~5% concentration, is adsorbed on the casting skin of shell outer surface and remaining shellfish meat with removal; Clean the phase III and adopt washing, to remove the cleaning agent and the residual contaminants of shell surface; Above three phases all adopts the rotary drum-type cleaning equipment, and utilizing between shell collides each other, rubs removes shell surface adsorbate, pollutant;
2. oven dry: the shell of 1. washing through step will carry out drying to remove moisture by drying plant behind draining; Want strict control bake out temperature to be no more than 85 ℃ during oven dry; Too high and the sex change of the active ingredient Yin Wendu that prevents shell, drying plant adopts band drier or cylindrical drier;
3. elementary pulverizing: elementary pulverizing is carried out in two steps; At first will pass through cleaning, the oven dry after the shell raw material pulverizing process the shell particle that particle diameter is 2~5mm; Shell particle with this 2~5mm continues to pulverize then, and obtaining particle diameter is the shell powder of 250 μ m~841 μ m;
4. fine powder is pulverized: the 3. middle shell powder through elementary pulverizing of step is carried out further grinding and processing through impact type micro mist pulverizer, obtain the shell powder of particle diameter at 5~15 μ m;
5. micro mist is pulverized: further dwindle for making the shell powder granule; Need to adopt fluid bed supersonic airstream disintegrating apparatus that the shell powder is further processed; With step 4. in particle diameter be the shell powder material of 5~15 μ m through the supersonic airstream pulverization process, obtain the powder product that particle diameter is 0.5~5 μ m;
6. nanoscale powder processing: adopt the processing of planetary ball mill comminuting method; Can make powder reach nanoscale; Adopting 5. middle upper level 0.5~5 μ m powder of step is raw material, adds pure water raw material furnishing paste is carried out ball milling, and processing back product cut size can reach 40~100nm;
7. post-processed: according to the difference at oyster shell whiting body and function place, can adopt different manner of packings, be beneficial to storage, transportation and the use of manufactured goods.
2. the manufacturing approach of a kind of shell ultra micro powder according to claim 1 is characterized in that: described raw material shell is that oyster shell, Xiayi shellfish shell, scallop shell, mussel shell, conch shell base substance structure are one or more of marine organisms hard shell of calcium carbonate.
3. the manufacturing approach of a kind of shell ultra micro powder according to claim 1; It is characterized in that: described above-mentioned process requires cleaning, sealing; It is high hard, wear-resisting that the piece surface of device interior and oyster shell whiting raw material contact portion is wanted, not with raw material generation chemical reaction.
4. the manufacturing approach of a kind of shell ultra micro powder according to claim 1 is characterized in that: for the ultra micro powder that is applied to food, pharmaceuticals industry, should arrange white picking technology, carry out at 1. wash phase for the first time; To being that concentration of 2~5mm shell particle arrangement is that 5%~10% hydrochloric acid cleans through elementary pulverizing, particle diameter, soak time is 1 minute, drains the back and arranges washing, baking operation for the second time; And isolate residual impurity through cyclopneumatic separator, obtain clean more oyster shell whiting raw material, and then it is carried out following process.
5. the manufacturing approach of a kind of shell ultra micro powder according to claim 1 is characterized in that: the operating temperature of said baking stage and shredding stage can not be above 85 ℃.
6. the manufacturing approach of a kind of shell ultra micro powder according to claim 1; It is characterized in that: can also clean, wash the back at above-mentioned caustic soda in the described cleaning process and add pickling process; Wherein pickling process adopts the hydrochloric acid of 10%~15% concentration; Thoroughly to dispose the residual contaminants that is adsorbed on the shellfish surface, arrange washing to remove the shell surface cleaning fluid after the pickling again.
7. the manufacturing approach of a kind of shell ultra micro powder according to claim 1; It is characterized in that: be used for food, pharmaceutical field; Can adopt vacuum packaging, the nanoscale paste shell powder that adopts the planetary ball mill comminuting method to obtain can directly add in food, the medicine; Obtain dry nanoscale shell powder like needs, can adopt freeze drying equipment that the paste that contains pure water is carried out freeze drying, thereby obtain the shell dry powder of nanoscale.
CN2011101182183A 2011-05-09 2011-05-09 Manufacturing method for ultrafine shell powder Pending CN102773140A (en)

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CN103073038A (en) * 2013-01-23 2013-05-01 浙江大学 Preparation method of acid-modified superfine shell powder and product
CN103159246A (en) * 2013-04-15 2013-06-19 吉林化工学院 Light calcium carbonate produced by using shells
CN103284930A (en) * 2013-05-10 2013-09-11 周卫忠 Preparation method of pure natural talcum powder
CN103571235A (en) * 2013-10-28 2014-02-12 浙江大学舟山海洋研究中心 Preparation method of prismatic biological calcium carbonate
CN103585252A (en) * 2013-11-13 2014-02-19 苏州鹰皇药业有限公司 Ultrafine composite wall-breaking method for directly-oral traditional Chinese medicine decoction pieces
CN103585950A (en) * 2013-12-02 2014-02-19 浙江海洋学院 Preparation method of natural shell adsorbent
CN103920574A (en) * 2013-01-11 2014-07-16 张仁鸿 Method for micronization of material having human body far-infrared ray wave band
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CN104256654A (en) * 2014-09-08 2015-01-07 程梅雪 Water-flowing type processing process of clam shells
CN104259131A (en) * 2014-09-08 2015-01-07 程梅雪 Clam shell cleaning, grinding and drying assembly line type manufacturing technology
CN104353637A (en) * 2014-09-08 2015-02-18 程梅雪 Cluster-type clam shell powder processing technology
CN104770562A (en) * 2015-03-23 2015-07-15 嵊泗县绿贻贝壳生态开发有限公司 Shell utilization method
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CN105901457A (en) * 2016-05-24 2016-08-31 辽宁佰福药业有限公司 Method for preparing oyster shell powder functional drink and drink and application thereof
CN106395876A (en) * 2016-08-26 2017-02-15 青岛食安生物工程有限公司 Process for preparing purely-natural nano supermicro calcium powder
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CN106900535A (en) * 2016-12-30 2017-06-30 浙江海洋大学 The extensive breeding apparatus of porphyra haitanensis shell conchocelis
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CN111534155A (en) * 2020-05-06 2020-08-14 秦皇岛美博士新型材料科技有限公司 Preparation method for preparing high-quality shell powder by utilizing waste shells
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CN103073038A (en) * 2013-01-23 2013-05-01 浙江大学 Preparation method of acid-modified superfine shell powder and product
CN103073038B (en) * 2013-01-23 2014-12-17 浙江大学 Preparation method of acid-modified superfine shell powder and product
CN103159246A (en) * 2013-04-15 2013-06-19 吉林化工学院 Light calcium carbonate produced by using shells
CN103159246B (en) * 2013-04-15 2016-08-10 吉林化工学院 Shell is utilized to produce precipitated calcium carbonate
CN103284930A (en) * 2013-05-10 2013-09-11 周卫忠 Preparation method of pure natural talcum powder
CN103571235B (en) * 2013-10-28 2015-12-30 浙江大学舟山海洋研究中心 A kind of preparation method of prismatic biological calcium carbonate
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CN103585252A (en) * 2013-11-13 2014-02-19 苏州鹰皇药业有限公司 Ultrafine composite wall-breaking method for directly-oral traditional Chinese medicine decoction pieces
CN103585950A (en) * 2013-12-02 2014-02-19 浙江海洋学院 Preparation method of natural shell adsorbent
CN104026652A (en) * 2014-02-28 2014-09-10 国家海洋局第三海洋研究所 Preparing method of food grade marine-organism-sourced shell micro powder
CN104256654A (en) * 2014-09-08 2015-01-07 程梅雪 Water-flowing type processing process of clam shells
CN104256654B (en) * 2014-09-08 2015-12-02 程梅雪 Continuous-flow type clam shell processing technology
CN104353637A (en) * 2014-09-08 2015-02-18 程梅雪 Cluster-type clam shell powder processing technology
CN104259131B (en) * 2014-09-08 2016-07-06 程梅雪 Conch Meretricis seu Cyclinae shell cleans, pulverizes, dries continuous-flow type preparation technology
CN104259131A (en) * 2014-09-08 2015-01-07 程梅雪 Clam shell cleaning, grinding and drying assembly line type manufacturing technology
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CN113881249A (en) * 2021-11-24 2022-01-04 吴振清 Oyster shell powder composite filler with super-hydrophobicity and preparation method thereof

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