CN109157871A - A method of the suspension containing stickum is separated by solid-liquid separation - Google Patents

A method of the suspension containing stickum is separated by solid-liquid separation Download PDF

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Publication number
CN109157871A
CN109157871A CN201811154249.2A CN201811154249A CN109157871A CN 109157871 A CN109157871 A CN 109157871A CN 201811154249 A CN201811154249 A CN 201811154249A CN 109157871 A CN109157871 A CN 109157871A
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solid
suspension containing
chitosan
liquid separation
separated
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CN109157871B (en
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刘爱青
王海燕
刘爽
刘利格
聂敬全
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Beijing Semnl Biotechnology Co ltd
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Anhui Shengmino Biotechnology Co Ltd
BEIJING SEMNL BIOTECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01Separation of suspended solid particles from liquids by sedimentation using flocculating agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The present invention provides a kind of methods being separated by solid-liquid separation to the suspension containing stickum, it is characterized in that, method includes the following steps: the suspension containing stickum is added in container under (1) stirring, chitosan and/or chitosan derivatives are added to the container at the same time;(2) after step (1), silica gel is added to the container.Method of the invention is greatly facilitated feed clarification process, so that precipitating is become more closely knit, to accelerate to be separated by solid-liquid separation by selecting suitable flocculant component and order of addition;For example, suspension separation time can shorten to about 5 hours from about 10 hours, or even by 2.5 hours.In addition, also further shortening separation of solid and liquid process, and improve the rate of recovery by the selection of the parameters such as the concentration of pH value to the solution being separated by solid-liquid separation, temperature, concentration and some specific flocculants;For example, the rate of recovery can be increased at least about 90%, up to 97.5% from about 75%%.

Description

A method of the suspension containing stickum is separated by solid-liquid separation
Technical field
The present invention relates to a kind of methods being separated by solid-liquid separation to the suspension containing stickum.
Background technique
Animal vegetable tissue extract usually contains the stickums such as protein, polysaccharide.They are the substances for being not readily dissolved in water, Colloidal solid dispersion is formd in aqueous solution;They are often with charge, due to the principle that identical charges repel each other, these colloids Particle cannot mutually be assembled, so being also difficult to separate from solution, cause solution muddy.Use conventional filter method with Clear solution is obtained, it is usually ineffective;And filtration time is long, such as tens hours, and the substance of filtering is easy to cause to become Matter.
For accelerated filtration process, this field is usually added into flocculant, to promote feed clarification, when so as to shorten filtering Between.For example, in the art, it is very common that flocculant chitosan or polyacrylamide, which is added, to promote feed clarification. But since the molecular weight of chitosan is smaller, the conglomeration for flocculating out in flocculation process is relatively fine, and sinking speed is slower, Even generally requiring tens hours of ten a few houres, make the inefficiency of clarified separation;Moreover, when being separated by solid-liquid separation, it is tiny Floc sedimentation is easy to float, and causes to return turbid phenomenon, also further increases the difficulty of separation of solid and liquid.Polyacrylamide is for containing The clarifying effect of the suspension of stickum is very unsatisfactory, often undergoes the very long time, and upper layer is still more muddy.
Patent of invention content
The present invention provides a kind of be easy to the suspension progress containing stickum to overcome above-mentioned technological deficiency The method of separation of solid and liquid.
The present invention provides a kind of methods being separated by solid-liquid separation to the suspension containing stickum, which is characterized in that Method includes the following steps:
(1) suspension containing stickum is added in container under stirring, it is poly- to container addition shell at the same time Sugar and/or chitosan derivatives;
(2) after step (1), silica gel is added to the container.
Feed clarification is greatly facilitated by selecting suitable flocculant component and order of addition in method of the invention Journey makes precipitating become more closely knit, to accelerate to be separated by solid-liquid separation;For example, suspension separation time can be shortened to from about 10 hours About 5 hours, or even by 2.5 hours.In addition, also by pH value to the solution being separated by solid-liquid separation, temperature, concentration and The selection of the parameters such as the concentration of some specific flocculants, further shortens separation of solid and liquid process, and improve the rate of recovery;Example Such as, the rate of recovery can be increased at least about 90%, up to 97.5% from about 75%.
Specific embodiment
The present invention provides a kind of methods being separated by solid-liquid separation to the suspension containing stickum, which is characterized in that Method includes the following steps:
(1) suspension containing stickum is added in container under stirring, adds shell to the container at the same time
Glycan and/or chitosan derivatives;
(2) after step (1), silica gel is added to the container.
The silica gel, the chitosan and the chitosan derivatives are not particularly limited, and commercially available silica gel, shell are poly- The purpose of the present invention may be implemented in the sugared and described chitosan derivatives.
The suspension containing stickum especially animality tissue enzymolysis liquid, more particularly oyster enzymolysis liquid.
In general, in order to clarify the suspension containing stickum containing anion insoluble matter, the chitosan derivatives Preferably cationic derivation object, such as may is that carboxymethyl chitosan, hydroxyethyl chitosan, carboxymethyl chitosan, chitosan Quaternary ammonium salt, chitosan hydrochloride etc..
Preferably, the water solubility of the chitosan derivatives is greater than the water solubility of the chitosan, such as may is that carboxylic first Base enclosure glycan, hydroxypropyl chitosan and chitosan hydrochloride etc..
In step (1), chitosan is selected perhaps chitosan derivatives or chitosan to be applied in combination and chitosan spreads out Biology, the content depending on required clear the suspension small molecular containing stickum and macromolecular insoluble matter.For example, The content of the insoluble matter of small molecule is higher, then selects the composition containing chitosan derivatives;Contain chitosan conversely, then using Composition.
In order to improve solid-liquid separation efficiency, it is preferable that in step (1), the suspension containing stickum and institute The weight ratio for stating chitosan/or the chitosan derivatives is 20000:1-8, preferably 20000:1.5-5;Or described contain The weight ratio of the total weight of the suspension of stickum and the chitosan and the chitosan derivatives is 20000:1-8, excellent It is selected as 20000:1.5-5.
Preferably, in step (2), the weight ratio of the suspension containing stickum and the silica gel is 5000: 1-30, preferably 5000:3-25.
In order to further increase solid-liquid separation efficiency, it is preferable that the temperature of the suspension containing stickum is 25- 85 DEG C, preferably 50-60 DEG C;The pH of the suspension containing stickum is 3-7, preferably 4.5-6;It is described to contain toughness The material concentration of the suspension of substance is in 2-10 weight %, preferably 5-8 weight %.
In order to improve solid-liquid separation efficiency, it is preferable that between step (1) and step (2), also under stiring to the appearance Device adds the step of gelatin.
In order to improve solid-liquid separation efficiency, it is preferable that the weight of the suspension containing stickum and the gelatin Than for 200000:1-8, preferably 200000:1.5-5.
In order to improve solid-liquid separation efficiency, it is preferable that after step (2), the chitosan is added into supernatant;It is preferred that The weight ratio of ground, the weight of the supernatant and the chitosan is 40000:1-8, preferably 40000:2-5.
In order to improve solid-liquid separation efficiency, it is preferable that after step (2), under stiring, be first added into transition zone inorganic Then polyacrylamide is added in flocculant.
The inorganic flocculating agent can be type commonly used in the art, such as can for aluminium polychloride, bodied ferric sulfate, Poly- sial, poly- ferrosilicon, poly- phosphorus aluminium, poly- ferrophosphorus.In a preferred embodiment, the inorganic flocculating agent is polyaluminium Aluminium.
In order to improve solid-liquid separation efficiency, it is preferable that the weight ratio of the transition zone and the inorganic flocculating agent is 100- The weight ratio of 1000:1, preferably 500-1000:1, the transition zone and the polyacrylamide is 10000-50000:1, excellent It is selected as 20000-30000:1.
In order to improve solid-liquid separation efficiency, it is preferable that the chitosan is configured to the molten of 0.1~3 weight % with organic acid Liquid;Preferably, the organic acid is selected from one or more of lactic acid, citric acid, acetic acid, oxalic acid.
Embodiment 1
Separation of solid and liquid process
(1) in the case where revolving speed is 50 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (is provided simultaneously to storage tank addition shell is poly- by the positive day in Tianjin at clarification technique Co., Ltd, 4kg shell Glycan acetic acid configuration concentration is 2 weight %).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 4.5, and temperature is 50 DEG C, and oyster is solid The concentration of shape object is 10 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 30kg silica gel is quickly added into storage tank Company provides).After standing 2.5 hours, solution layering.Collection obtains the supernatant of 18000kg.
Embodiment 2
Separation of solid and liquid process
(1) in the case where revolving speed is 15 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (is provided simultaneously to storage tank addition chitosan by the positive day in Tianjin at clarification technique Co., Ltd, 2kg Chitosan acetic acid configuration concentration is 1 weight %).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 6, and temperature is 60 DEG C, and oyster is solid The concentration of shape object is 6 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 100kg silica gel is quickly added into storage tank Company provides).After standing 4 hours, solution layering.Collect the transition zone of the supernatant and 1200kg that obtain 18500kg.
(3) in the case where revolving speed is 15 revs/min of stirring, chitosan is added into above-mentioned supernatant (by the positive day of saliva at clarification skill Art Co., Ltd provides, and 2kg chitosan acetic acid configuration concentration is 1 weight %).After standing 0.5 hour, solution layering.It receives Collection obtains the supernatant of 18000kg.
(4) in the case where revolving speed is 15 revs/min of stirring, the poly- of 12kg is added into the transition zone of step (2) acquisition first Aluminium chloride (configuration concentration be 3/1000ths aqueous solution) is closed, then adding the polyacrylamide of 0.06kg, (configuration concentration is 3/1000ths aqueous solution).After standing 1 hour, solution layering.Collection obtains the supernatant of 800kg.
Embodiment 3
Separation of solid and liquid process
(1) in the case where revolving speed is 40 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and simultaneously to the storage tank addition chitosan solution (by the positive day in Tianjin at clarification technique Co., Ltd provide, 1.5kg chitosan acetic acid configuration concentration is 1 weight %).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.2, temperature 60 DEG C, the concentration of oyster solid content is 2 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 75kg silica gel is quickly added into storage tank Company provides).After standing 2 hours, solution layering.Collect the transition zone of the supernatant and 1500kg that obtain 17500kg.
(4) in the case where revolving speed is 35 revs/min of stirring, the poly- of 1.5kg is added into the transition zone of step (2) acquisition first Ferric sulfate (configuration concentration be 3/1000ths aqueous solution) is closed, then adding the polyacrylamide of 0.15kg, (configuration concentration is 3/1000ths aqueous solution).After standing 0.5 hour, solution layering.Collection obtains the supernatant of 1200kg.
Embodiment 4
Separation of solid and liquid process
(1) in the case where revolving speed is 50 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (is provided simultaneously to storage tank addition chitosan by the positive day in Tianjin at clarification technique Co., Ltd, 3kg Chitosan acetic acid configuration concentration is 0.5 weight %), when feed liquid discharging is to half, to storage tank addition gelatin (by French sieve Celo company provides, and 3kg gelatin is formulated as 1 weight % with deionized water).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.2, Temperature is 60 DEG C, and the concentration of oyster solid content is 5 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 20kg silica gel is quickly added into storage tank Company provides).After standing 4 hours, solution layering.Collect the transition zone of the supernatant and 1200kg that obtain 18000kg.
(3) in the case where revolving speed is 45 revs/min of stirring, chitosan is added into above-mentioned supernatant (by the positive day of saliva at clarification skill Art Co., Ltd provides, and it is 1 weight % that 0.5kg chitosan, which is configured to concentration with acetic acid).After standing 1 hour, solution layering. Collection obtains the supernatant of 17800kg.
(4) in the case where revolving speed is 35 revs/min of stirring, the poly- of 6.5kg is added into the transition zone of step (2) acquisition first Aluminium chloride (concentration be 3/1000ths aqueous solution) is closed, then adding the polyacrylamide of 0.075kg, (concentration is 3/1000ths Aqueous solution).After standing 0.6 hour, solution layering.Collection obtains the supernatant of 1000kg.
Embodiment 5
Separation of solid and liquid process
(1) in the case where revolving speed is 40 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and simultaneously to the storage tank addition chitosan solution (by the positive day in Tianjin at clarification technique Co., Ltd provide, It is 1 weight % that 5kg chitosan, which is configured to concentration with acetic acid).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.2, temperature 60 DEG C, the concentration of oyster solid content is 8 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 50kg silica gel is quickly added into storage tank Company provides).After standing 3.5 hours, solution layering.Collect the transition zone of the supernatant and 1300kg that obtain 18500kg.
(4) in the case where revolving speed is 35 revs/min of stirring, the poly- of 3.5kg is added into the transition zone of step (2) acquisition first Ferric sulfate (concentration be 3/1000ths aqueous solution) is closed, then adding the polyacrylamide of 0.045kg, (concentration is 3/1000ths Aqueous solution).After standing 0.5 hour, solution layering.Collection obtains the supernatant of 800kg.
Embodiment 6
Separation of solid and liquid process
(1) in the case where revolving speed is 40 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (is had simultaneously to storage tank addition chitosan and chitosan derivatives by the positive day in Tianjin at clarification technique Limit company provides, and it is 1 weight % that wherein 2kg chitosan, which is configured to concentration with acetic acid,;2kg chitosan derivatives are matched with deionized water It is set to 1 weight %);Wherein, chitosan is first added, adds chitosan derivatives later.Wherein, the pH value of oyster enzymatic hydrolysis suspension It is 5.2, temperature is 60 DEG C, and the concentration of oyster solid content is 3 weight %.
(2) after step (1), 37.5kg silica gel is quickly added into storage tank (is had by Shenzhen's grand plan silica gel science and technology Limit company provides).After standing 2 hours, solution layering.Collect the transition zone of the supernatant and 1300kg that obtain 18500kg.
(4) in the case where revolving speed is 45 revs/min of stirring, the polymerization of 6kg is added into the transition zone of step (2) acquisition first Aluminium chloride (concentration be 3/1000ths aqueous solution), then adding the polyacrylamide of 0.065kg, (concentration is 3/1000ths Aqueous solution).After standing 0.5 hour, solution layering.Collection obtains the supernatant of 900kg.
Embodiment 7
Separation of solid and liquid process
(1) in the case where revolving speed is 50 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (is mentioned simultaneously to storage tank addition chitosan derivatives by the positive day in Tianjin at clarification technique Co., Ltd For 4kg chitosan derivatives are configured to 1 weight % with deionized water).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.2, temperature Degree is 60 DEG C, and the concentration of oyster solid content is 4 weight %.
(2) after step (1), it is (limited by Shenzhen's grand plan silica gel science and technology that 65kg silica gel is quickly added into storage tank Company provides).After standing 3 hours, solution layering.Collect the transition zone of the supernatant and 1000kg that obtain 18700kg.
(4) in the case where revolving speed is 50 revs/min of stirring, the polymerization of 4kg is added into the transition zone of step (2) acquisition first Aluminium chloride (concentration be 3/1000ths aqueous solution), then adding the polyacrylamide of 0.08kg, (concentration is 3/1000ths Aqueous solution).After standing 0.4 hour, solution layering.Collection obtains the supernatant of 800kg.
Comparative example 1
(1) in the case where revolving speed is 50 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and simultaneously to the storage tank addition chitosan solution (by the positive day in Tianjin at clarification technique Co., Ltd provide, 24kg chitosan acetic acid configuration concentration is 1 weight %).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.2, and temperature is 60 DEG C, The concentration of oyster solid content is 4 weight %.After standing 10 hours, solution layering.Collection obtains the supernatant of 15000kg.
Comparative example 2
(1) in the case where revolving speed is 50 revs/min of stirring, by 20 tons of oyster enzymatic hydrolysis suspension with the charging of 0.5 tonnes per minute clock Speed is pumped into storage tank, and (by the 1.2kg of Ai Sen company, uses deionized water to storage tank addition polyacrylamide solution simultaneously It is configured to 0.2 weight %).Wherein, the pH value of oyster enzymatic hydrolysis suspension is 5.0, and temperature is 80 DEG C, and the concentration of oyster solid content is 3 weight %.After standing 8 hours, though solution has layering, upper layer is still more muddy, can not be separated by solid-liquid separation.

Claims (10)

1. a kind of method being separated by solid-liquid separation to the suspension containing stickum, which is characterized in that this method includes following Step:
(1) stir under the suspension containing stickum is added in container, at the same time to the container addition chitosan and/ Or chitosan derivatives;
(2) after step (1), silica gel is added to the container.
2. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein in step (1) in, the suspension containing stickum is 20000 with the weight ratio of the chitosan/or the chitosan derivatives: 1-8, preferably 20000:1.5-5;Or the suspension containing stickum spreads out with the chitosan and the chitosan The weight ratio of the total weight of biology is 20000:1-8, preferably 20000:1.5-5.
3. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein in step (2) in, the weight ratio of the suspension containing stickum and the silica gel is 5000:1-30, preferably 5000:3-25.
4. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein described to contain The temperature of the suspension of toughness substance is 25-85 DEG C, preferably 50-60 DEG C;The pH of the suspension containing stickum For 3-7, preferably 4.5-6;The material concentration of the suspension containing stickum is in 2-10 weight %, preferably 5-8 weight Measure %.
5. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein in step (1) between step (2), also under stiring to the container add gelatin the step of.
6. the method according to claim 5 being separated by solid-liquid separation to the suspension containing stickum, wherein described to contain The weight ratio of the suspension of toughness substance and the gelatin is 200000:1-8, preferably 200000:1.5-5.
7. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein in step (2) after, the chitosan is added into supernatant;Preferably, the weight of the supernatant and the weight ratio of the chitosan are 40000:1-8.
8. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein in step (2) after, under stiring, inorganic flocculating agent is first added into transition zone, polyacrylamide is then added;The inorganic flocculating agent is excellent It is selected as aluminium polychloride, bodied ferric sulfate, poly- sial, poly- ferrosilicon, poly- phosphorus aluminium, poly- ferrophosphorus.
9. the method according to claim 8 being separated by solid-liquid separation to the suspension containing stickum, wherein the mistake The weight ratio of layer and the inorganic flocculating agent is crossed as 100-1000:1, preferably 500-1000:1, the transition zone gathers with described The weight ratio of acrylamide is 10000-50000:1, preferably 20000-30000:1.
10. the method according to claim 1 being separated by solid-liquid separation to the suspension containing stickum, wherein described Chitosan is configured to the solution of 0.1~3 weight % with organic acid;Preferably, the organic acid be selected from lactic acid, citric acid, acetic acid, One or more of oxalic acid.
CN201811154249.2A 2018-09-30 2018-09-30 Method for carrying out solid-liquid separation on suspension containing viscous substances Active CN109157871B (en)

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CN102321686A (en) * 2011-09-14 2012-01-18 中粮生物化学(安徽)股份有限公司 Processing method and application of starch raw material
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