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WO2017148343A1 - Procédé de recyclage de coquille d'œuf et utilisations de matériau recyclé - Google Patents

Procédé de recyclage de coquille d'œuf et utilisations de matériau recyclé Download PDF

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Publication number
WO2017148343A1
WO2017148343A1 PCT/CN2017/074955 CN2017074955W WO2017148343A1 WO 2017148343 A1 WO2017148343 A1 WO 2017148343A1 CN 2017074955 W CN2017074955 W CN 2017074955W WO 2017148343 A1 WO2017148343 A1 WO 2017148343A1
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WO
WIPO (PCT)
Prior art keywords
eggshell
powder
membrane
hydrolysis
recycling method
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2017/074955
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English (en)
Chinese (zh)
Inventor
梁玮彤
刘佩诗
朱景基
何嘉仪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
World Houseware Producing Co Ltd
Original Assignee
World Houseware Producing Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by World Houseware Producing Co Ltd filed Critical World Houseware Producing Co Ltd
Publication of WO2017148343A1 publication Critical patent/WO2017148343A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
    • B09B3/35—Shredding, crushing or cutting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/60—Biochemical treatment, e.g. by using enzymes

Definitions

  • the present invention belongs to the field of waste recycling, and specifically relates to the recovery of an eggshell and the use of recycled materials.
  • the egg consists of egg yolk, egg white, two-layer eggshell membrane and eggshell. Eggs are used as frequent visitors on each table. The consumption is very large. After cooking egg yolk and egg white, the rest is generally treated as waste. Recycling, but in fact, the value of the eggshell is underestimated as waste material, Osuoji et al reported that acidic glycosaminoglycans are present in the eggshell membrane, and glycosaminoglycans (ie, hyaluronic acid) may be used for water retention and against bacterial attack, more studies have reported that eggshell membranes contain many valuable compounds, such as cross-linked collagen (1, V and X), glycosaminoglycans (ie hyaluronic acid, chondroitin sulfate, Heparan sulfate and keratan sulfate), egg white proteins (eg, ovotransferrin, lysozyme) and eggshell matrix proteins (eg egg calcium)
  • FIG. 1 shows a cross-sectional view of the eggshell without the use of the present invention provided by the conventional comminution, eggshell membrane removal, rinsing and drying after removal of the inner and outer membrane shells.
  • the outer eggshell membrane (1) has a tip of the milk cone (2) similar to the fiber penetrating the eggshell, and the recovery is not complete.
  • useful components such as calcium carbonate, eggshell membrane powder (containing protein, collagen, elastin, hyaluronic acid)
  • recovers the most abundant useful calcified eggshell powder containing calcium carbonate and can increase the extraction from the egg
  • the shell and eggshell membranes are then dried into eggshell membrane powders of valuable organic contents such as protein, collagen, elastin, and hyaluronic acid
  • the method provided by the present invention is as follows:
  • An eggshell waste recycling method comprising the following steps:
  • the particle size of the eggshell after pulverization is less than or equal to 2000 micrometers, preferably 0.1 to 99 micrometers, and the smaller the particle size of the eggshell waste, the larger the hydrolysis contact area in the hydrolysis process, and the more the hydrolysis process Short, the extraction efficiency is higher;
  • a suitable particle size can be reduced before the start of the hydrolysis reaction, ie, before the start of step (3), such as the crushed eggshell in step (2), which is an effective way, the eggshell particles The size does not substantially change in the hydrolysis reaction.
  • hydrolysis is carried out with a membrane eggshell powder, an enzyme and a buffer having a weight ratio ranging from 70:0.125:1000 to 150:11:2000, and the preferred hydrolysis temperature is about 20-60.
  • the preferred hydrolyzed crucible is about 1-24 hours, the preferred stirring speed is about 350-1000 rpm, and the pH of the buffer can be any suitable pH that matches the enzyme used. , preferred pH It is 1-8, and after hydrolysis, an organic substance similar to a liquid phase and an inorganic substance which is not hydrolyzed are obtained;
  • a more preferred hydrolysis temperature is about 20-37 degrees Celsius
  • a more preferred hydrolyzed crucible is about 1-3 hours
  • the weight ratio of the membrane eggshell powder, the enzyme and the buffer is between 70:0.25:1000 and 70:0.5:1000;
  • a more preferred agitation speed is between about 550 and 1000 rpm;
  • the buffer is PBS Phosphate-buffered saline, TAE buffer or TBE buffer;
  • the hydrolysis reaction can be passed through the continuous pulverization stirring system.
  • the hydrolysis reaction can be passed through the continuous pulverization stirring system.
  • the hydrolyzed contact area of the filmed eggshell powder including but not limited to homogenizers, continuous ultrasonic reactors or others containing agitation and homogenization or chopping or grinding or grinding to achieve sustained A reactor/container with reduced particle size, by which the total length of the entire hydrolysis process is shortened.
  • the enzyme used in the hydrolysis in the step (3) is one or more proteases having at least one thiol group, such as kiwi protease, bromelain, ficin, papain, pepsin or ginger protease, single thiol protease or sulfhydryl group.
  • the combination of proteases is used for specific enzymatic hydrolysis to increase the solubility of organic contents extracted from eggshell waste (both eggshell and eggshell membranes) without extensive digestion of valuable organic content.
  • the method used in the separation in the step (4) includes a suction filtration separation and a pressure filtration separation, and the suction filtration separation and the pressure filtration separation may be performed at room temperature using a filtration membrane, preferably a pore size filter of 5-11 micrometers. membrane.
  • the method used in the separation in the step (4) is centrifugal separation, and the centrifugal separation is preferably performed at room temperature by using at least 5000 rpm.
  • the drying methods in steps (5) and (6) are spray drying and freeze drying, spray drying inlet temperature Preferably, it is 95-140 degrees Celsius, more preferably the inlet temperature is 95-115 degrees Celsius; the preferred suction rate is about 50 ⁇ 3 ⁇ 4-90%, and the more preferred suction rate is about 60-70%; the preferred pump speed is about 10-50%, more preferably 20-30%; freeze-drying preferably is between -30 degrees Celsius and 20 degrees Celsius under vacuum, more preferably 8-13 degrees Celsius under vacuum.
  • the recovery method further comprises the steps of: dissolving the eggshell membrane powder, separating, purifying, and drying to obtain sodium hyaluronate, the purity of which is up to 90% or more.
  • Sodium hyaluronate is a biochemical drug with high clinical value and is widely used in various ophthalmic operations, such as crystal implantation, corneal transplantation and anti-glaucoma surgery. It can also be used to treat arthritis and accelerate wound healing. It is used in cosmetics and can play a unique role in protecting the skin. It can keep the skin moist and smooth, delicate and tender, elastic, anti-wrinkle, anti-wrinkle, beauty care and restore skin physiological function.
  • the eggshell powder prepared by the above method used to replace the existing calcium carbonate filler to prepare a thermoplastic
  • the eggshell powder obtained by the method has a particle size of less than or equal to 800 micrometers, and can reach 0.1. -45 microns, and a calcium carbonate content of 90% to 99%, with little or no organic content, can be used in place of existing calcium carbonate polymer fillers to be incorporated into thermoplastic products using single or twin screw extruders.
  • thermoplastic is prepared by using polyethylene, polylactic acid, polypropylene, poly(ethylene vinyl acetate) or/and polyvinyl chloride and the eggshell powder prepared by the present invention, wherein the eggshell powder It is 15% to 60% by weight and may contain other additive components such as antimicrobials, antistatic agents, coupling agents, dyes and pigments, fillers, flame retardants, foaming agents, heat stabilizers, and A nucleating agent, an odor releasing agent, an ultraviolet ray or a light stabilizer, the thermoplastic polymer composite can be further processed by extrusion, injection molding, blow molding, and fused deposition molding to form a thermoplastic product.
  • additive components such as antimicrobials, antistatic agents, coupling agents, dyes and pigments, fillers, flame retardants, foaming agents, heat stabilizers, and A nucleating agent, an odor releasing agent, an ultraviolet ray or a light stabilizer
  • FIG. 1 is a cross-sectional view of an eggshell powder after separation of an eggshell membrane by a conventional method under a scanning electron microscope;
  • FIG. 2 is a process flow diagram of the present application;
  • Example 3 is a cross-sectional view of the filmed eggshell powder after hydrolysis in Example 1 under a scanning electron microscope;
  • FIG. 4 is a graph showing the relationship between the protein size and the main particle size of the eggshell powder per gram of eggshell;
  • FIG. 5 is a comparison chart of particle size distribution before and after hydrolysis of Example 2; [0036] FIG.
  • FIG. 6 is a comparison chart of particle size distribution before and after hydrolysis of Example 3.
  • Example 7 is a cross-sectional view of an electron microscope of the eggshell powder hydrolyzed by Example 4.
  • FIG. 8 is an analysis diagram of a solid phase eggshell powder treated with a membrane eggshell, an eggshell membrane, and a ficin protease by a Fourier transform infrared spectrometer;
  • Example 9 is a cross-sectional view of the filmed eggshell powder after hydrolysis in Example 5 under an electron microscope;
  • FIG. 10 is a polymer filler particle having an eggshell powder content of 30% by volume and polyethylene mixed in different particle size ranges;
  • FIG. 11 is an eggshell powder having a particle size ranging from 22 to 45 micrometers, which is different A polymer filler in which the content is separately mixed with polyethylene.
  • an eggshell waste recycling method comprises the following steps: [0045] (1) selecting the recovered membrane eggshell, and rinsing the eggshell with sterile water for 3 minutes Removing dirt and microorganisms; (2) pulverizing the eggshell with a grind to increase its specific surface area, and pulverizing the eggshell to have a particle diameter of 2000 ⁇ m or less to obtain a filmed eggshell powder;
  • the liquid phase is taken, and the eggshell membrane powder is obtained after drying; the solid phase is taken, and dried at 80 ° C to obtain eggshell powder.
  • FIG. 3 shows the surface of the eggshell after the hydrolysis process in the present example under a scanning electron microscope.
  • the outer eggshell membrane is inserted into the eggshell's milk cone (2).
  • the similar fiber at the tip disappears, indicating that the enzymatic hydrolysis has been substantially completed.
  • FIG. 4 shows that as the particle size of most of the recovered membrane eggshells decreases, the extracted protein content increases.
  • reaction mixture was stirred with an overhead electronic stirrer at 1000 rpm;
  • the solid phase was obtained, and the eggshell powder was obtained after drying at 80 ° C, and the obtained eggshell powder was subjected to particle size analysis by using a vibrating screen.
  • FIG. 5 shows that the particle size distribution after the pulverization of the membrane eggshell is not changed in the reaction of the present embodiment, and the reaction
  • the particle size was basically unchanged after (hydrolysis) and after 24 hours of reaction.
  • the hydrolyzed material is subjected to solid-liquid centrifugation, centrifuged at 5000 rpm for 3 minutes at room temperature to obtain a solid phase, and dried at 80 ° C to obtain eggshell powder, and the obtained eggshell powder is passed.
  • a particle size analysis was performed using a vibrating screen.
  • Figure 6 shows that after hydrolysis by Example 3, most of the solid particles above 315 microns were reduced to about 22 microns.
  • the resulting eggshell membrane powder contains protein At about 60 ppm, containing hyaluronic acid of about 18.7 ppm;
  • (6) After separation by suction filtration, the solid phase is obtained, and the eggshell powder is obtained after drying at 80 ° C, and the eggshell powder is taken and characterized by an electron microscope (Fig. 7).
  • Fig. 7 shows the embodiment. An electron microscopic cross-sectional view of the hydrolyzed eggshell powder, no similar fibers were found inserted from the outer eggshell membrane into the tip of the milk cone (2) of the eggshell, and most of the solid particle size did not change in this example. .
  • lyophilization taking the liquid phase, lyophilizing to obtain eggshell membrane powder, lyophilization is under vacuum, 10 degrees Celsius
  • the final protein content per gram of membrane eggshell powder is 7.50 mg
  • sodium hyaluronate is 35.68 ⁇ ⁇
  • elastin is 0.0812.
  • FIG. 9 is a cross-sectional view showing an eggshell of the eggshell subjected to the hydrolysis process of Example 5, and no similar fibers of the tip of the milk cone (2) inserted from the outer eggshell membrane into the eggshell were found, most of which were 315 ⁇ m or more.
  • the solid particles are reduced to more than 22 microns.
  • Example 2 After the six steps in Example 1, the obtained eggshell powder was subjected to X-ray fluorescence analysis, and the results showed that the calcium content was 92% or more.
  • the eggshell powder is then divided into different particle size ranges using a size sieve: 500-80 0 microns, 150-315 microns, 90-150 microns and 22-45 microns.
  • eggshell powders of different particle size ranges were respectively mixed with a polyethylene resin at a content of 30% to form a polymer filler at 150%.
  • the eggshell powder of the particle size range of 22-45 micrometers was respectively 15% by weight
  • Table 1 below shows the soluble proteins extracted by hydrolysis of brown eggshells with eggshell membranes using different proteases with at least one sulfhydryl group at different temperatures.
  • the extracted soluble proteins were quantified using Pierce BCA protein.
  • the extracted elastin was analyzed using MyBioSource's Elastin ELISA kit, and the extracted hyaluronic acid was analyzed using Corgenix's Hyaluronic acid ELISA kit.

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  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Cosmetics (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

L'invention concerne un procédé permettant de recycler complètement une coquille d'œuf et un film de coquille d'œuf. Sans séparer la coquille d'œuf du film de coquille d'œuf, des composants utiles sont extraits de déchets de coquille d'œuf qui ne sont pas séparés, de sorte que de la poudre de coquille d'œuf calcifiée utile contenant du carbonate de calcium soit recyclée et des contenus organiques de valeur extraits de la poudre de coquille d'œuf séchée puissent être augmentés. Dans le procédé, des coquilles d'œuf peuvent être recyclées et utilisées dans une mesure maximale; dans le cas où les coquilles d'œuf et les films de coquille d'œuf n'ont pas besoin d'être séparés, des matières organiques ne sont pas détruites au moyen d'un procédé d'hydrolyse enzymatique, et la partie organique et la partie inorganique sont séchées séparément de manière à obtenir des substances qui sont différentes dans des applications.
PCT/CN2017/074955 2016-03-02 2017-02-27 Procédé de recyclage de coquille d'œuf et utilisations de matériau recyclé Ceased WO2017148343A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/CN2016/075275 WO2017147796A1 (fr) 2016-03-02 2016-03-02 Procédé de recyclage de coquille d'œuf et son utilisation
CNPCT/CN2016/075275 2016-03-02

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WO2017148343A1 true WO2017148343A1 (fr) 2017-09-08

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PCT/CN2017/074955 Ceased WO2017148343A1 (fr) 2016-03-02 2017-02-27 Procédé de recyclage de coquille d'œuf et utilisations de matériau recyclé

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Publication number Priority date Publication date Assignee Title
CN107513448A (zh) * 2017-10-17 2017-12-26 陈远志 城市生活垃圾制作清洁固体燃料的方法
CN115382877A (zh) * 2022-08-15 2022-11-25 武汉新华扬生物股份有限公司 一种分离蛋壳与蛋壳膜的方法

Citations (7)

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CN103069000A (zh) * 2010-08-31 2013-04-24 天野酶株式会社 使用了酶的蛋壳膜的溶解方法
CN103302080A (zh) * 2013-06-27 2013-09-18 北京二商健力食品科技有限公司 一种蛋壳粉的制备方法及加工设备
CN103316896A (zh) * 2013-06-27 2013-09-25 北京二商健力食品科技有限公司 一种蛋壳粉的加工方法
JP2013233120A (ja) * 2012-05-10 2013-11-21 Domo Corporation:Kk 卵殻と卵殻膜との分離回収方法及び分離回収装置
US20150182598A1 (en) * 2011-08-03 2015-07-02 Molecular Biology International, Inc. Collagen mixture and method of making the same
CN105598138A (zh) * 2016-03-02 2016-05-25 世界家庭用具制品厂有限公司 一种蛋壳回收方法及其用途

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WO2006078824A2 (fr) * 2005-01-18 2006-07-27 Biova, L.L.C. Procede de separation de membrane de coquille d'oeuf
CN101649341A (zh) * 2009-09-04 2010-02-17 黄继红 一种从禽蛋壳膜中提取蛋白肽的方法
CN102743317A (zh) * 2011-04-19 2012-10-24 南通宏利达针织有限公司 从蛋壳中分离蛋壳膜的方法
CN103059606B (zh) * 2012-12-24 2014-10-08 暨南大学 一种含有天然生物钙化物的硬质复合颗粒材料及其制备方法与应用
CN103275205B (zh) * 2013-05-08 2014-12-03 江苏福旦生物医药有限公司 一种水溶性禽蛋膜活性肽生产方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005118607A1 (fr) * 2004-05-28 2005-12-15 Calcigen Corporation Production des hyaluronates
CN103069000A (zh) * 2010-08-31 2013-04-24 天野酶株式会社 使用了酶的蛋壳膜的溶解方法
US20150182598A1 (en) * 2011-08-03 2015-07-02 Molecular Biology International, Inc. Collagen mixture and method of making the same
JP2013233120A (ja) * 2012-05-10 2013-11-21 Domo Corporation:Kk 卵殻と卵殻膜との分離回収方法及び分離回収装置
CN103302080A (zh) * 2013-06-27 2013-09-18 北京二商健力食品科技有限公司 一种蛋壳粉的制备方法及加工设备
CN103316896A (zh) * 2013-06-27 2013-09-25 北京二商健力食品科技有限公司 一种蛋壳粉的加工方法
CN105598138A (zh) * 2016-03-02 2016-05-25 世界家庭用具制品厂有限公司 一种蛋壳回收方法及其用途

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