CN108624284A - A kind of technique preparing aqueous labeling agent using ultrasonic-microwave collaboration method - Google Patents

A kind of technique preparing aqueous labeling agent using ultrasonic-microwave collaboration method Download PDF

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CN108624284A
CN108624284A CN201810423540.9A CN201810423540A CN108624284A CN 108624284 A CN108624284 A CN 108624284A CN 201810423540 A CN201810423540 A CN 201810423540A CN 108624284 A CN108624284 A CN 108624284A
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labeling agent
ultrasonic
cetanol
microwave
coalescents
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CN108624284B (en
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汪涛
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CHUZHOU HAICHUAN PRINTING PACKAGING Co.,Ltd.
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汪涛
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J189/00Adhesives based on proteins; Adhesives based on derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Preparation (AREA)

Abstract

The invention discloses a kind of techniques preparing aqueous labeling agent using ultrasonic microwave collaboration method, are related to aqueous adhesive technical field, include the following steps:(1) pretreatment of gelatin, the chemical modification of (2) cetanol, the preparation of (3) coalescents, the preparation of (4) aqueous labeling agent.The made labeling agent of the present invention can quickly form ultra-thin bonding film in labeling between label and commodity, the formation of the bonding film both can guarantee firm attachment of the label under commodity normal operating condition, can guarantee to impregnate by clear water when commodity are recycled again can be effectively peeled off trade mark with backwashing manner and remove labeling agent, and labeling agent clearance rate is made to reach 99.5% or more.

Description

A kind of technique preparing aqueous labeling agent using ultrasonic-microwave collaboration method
Technical field:
The present invention relates to aqueous adhesive technical fields, and in particular to a kind of to prepare water using ultrasonic-microwave collaboration method Property labeling agent technique.
Background technology:
Label agent, i.e. Commercial goods labels adhesive.Currently, many recyclable commodity packagings are all individually carried out using adhesive The stickup of label, such as plastic packing product and glass packaging product, in order in recycling quickly into the stripping of row label.
Existing adhesive mainly uses traditional casein cement and aqueous composite adhesives, but both products all have one Fixed defect.First, traditional casein cement is temperature sensitive, when temperature reduces or increases, the viscosity meeting of casein cement It is rapidly rising or falling, influences the stability in use of product;And casein cement haves the shortcomings that high speed shear is thinning, in height The stability of product is poor when fast machine uses, and is easy to splash away from sizing idler wheel, causes the pollution of machine and a large amount of losses. Secondly, aqueous composite adhesives use a large amount of macromolecular waterproof resins as raw material, although solving the resistance to water problems of label, together When reduce temperature sensitivity, but since macromolecule resin is insoluble in water, recycled in plastic packing product or glass packaging product When adhesive residue can not clean up completely, if using cosolvent come remove adhesive residue again exist increase cleaning The problem of wastewater treatment difficulty.
Invention content:
Technical problem to be solved by the present invention lies in provide that a kind of raw material is easy to get, operation is simple and the feature of environmental protection is strong The technique for preparing aqueous labeling agent using ultrasonic-microwave collaboration method.
The technical problems to be solved by the invention are realized using technical solution below:
A kind of technique being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, is included the following steps:
(1) pretreatment of gelatin:Edible gelatin is added in the water of 5-10 times of weight, is dispersed with stirring and is uniformly placed on ultrasound In wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave power are set Hydrolysis of polymaleic anhydride is added after 700W, reflow treatment 5-10min, stirs evenly, continues reflow treatment 5-10min, gained is mixed It closes object and lotion is made through being concentrated under reduced pressure, lotion is sent into after cooled to room temperature in freeze drier, dry obtained solid warp Particle is made in pulverizer;
(2) chemical modification of cetanol:After cetanol and L-Glutimic acid are mixed plus absolute ethyl alcohol dissolves, then is added dropwise dense Sulfuric acid regulation solution pH value is heated to reflux state insulated and stirred to 4-5, stops heating after reaction, through being concentrated under reduced pressure Ethyl alcohol is recycled, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, and dry gained particle is through ultra micro Micro mist is made to get modified cetanol in pulverizer;
(3) preparation of coalescents:It is heated to after food-grade polyglutamic acid and PEG-60 rilanit specials are mixed 105-110 DEG C of insulated and stirred 5-10min, then with the cooling rate of 5 DEG C/min be cooled to 0-5 DEG C heat preservation stand 1-3h to get at Film auxiliary agent;
(4) preparation of aqueous labeling agent:Gelatin after pretreatment, coalescents and modified cetanol are added to the water, Stirring and dissolving is complete, and viscosity control is in 1000-3000mPa.s to get aqueous labeling agent.
Edible gelatin in the step (1), hydrolysis of polymaleic anhydride mass ratio be 100:1-10.
Cetanol in the step (2), L-Glutimic acid mass ratio be 10:5-10.
Food-grade polyglutamic acid in the step (3), PEG-60 rilanit specials mass ratio be 5:1-5.
Gelatin after pretreatment in the step (4), coalescents, modified cetanol mass ratio be 100:5-15: 1-10。
Coalescents also include the nanometer rubber powder with PEG-60 rilanit special equivalent, nanometer rubber powder in the step (3) Preparation method be:Brazil wax is added into polyethylene glycol oxide, and is heated to molten condition insulated and stirred, adds ultra-fine Nanometer powder is made to get nanometer rubber powder using nano-level grinder while hot after mixing in magnesia.
The polyethylene glycol oxide, Brazil wax, super fine magnesia mass ratio be 1-5:1-5:1-5.
The beneficial effects of the invention are as follows:
(1) present invention is using hydrolysis of polymaleic anhydride as pretreating agent, and cooperates with method significantly to change by ultrasonic-microwave The cold water-soluble of kind gelatin;Although ultrasonic-microwave collaboration is owned by France in ordinary skill in the art means, it is specifically answered It uses in the pretreatment of gelatin and the operation for obtaining improvement gelatin cold water-soluble technique effect is not belonging to skill customary in the art Art means;And although pretreating agent hydrolysis of polymaleic anhydride is in acidity, its with this field routine pretreatment inorganic acid or The physicochemical property of organic acid is entirely different, and this field does not disclose the technical side using hydrolysis of polymaleic anhydride as pretreating agent Case, and the common knowledge of this field does not provide the technical inspiration using hydrolysis of polymaleic anhydride as pretreating agent yet;
(2) present invention keeps made modified cetanol soluble easily in water by the chemical modification to cetanol, while utilizing spermaceti The emulsifiability that alcohol itself has is compatible to promote the blending that labeling agent prepares raw material;And made modified cetanol has certain Thickening property, to improve it is made labeling agent adhesive force;
(3) present invention by the preparation of coalescents with cooperate with gelatin and modified cetanol improve made labeling agent at Film properties, so that made labeling agent can quickly form ultra-thin bonding film, the bonding film in labeling between label and commodity Formation not only can guarantee firm attachment of the label under commodity normal operating condition, but also can guarantee and pass through clear water when commodity recycle Immersion and backwashing manner can be effectively peeled off trade mark and remove labeling agent, and labeling agent clearance rate is made to reach 99.5% or more;
(4) present invention further increases the use of made labeling agent by the additional addition of nanometer rubber powder in coalescents Performance enhances the synergistic effect of gelatin and coalescents using the distinctive penetrability of nanometer rubber powder and permeability.
Specific implementation mode:
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 5g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:It is heated after 5g food-grades polyglutamic acid and 4g PEG-60 rilanit specials are mixed To 105-110 DEG C of insulated and stirred 5min, then 0-5 DEG C of heat preservation standing 1h is cooled to the cooling rate of 5 DEG C/min and is helped to get film forming Agent;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 8g coalescents and 5g modification cetanol are added Enter in water, stirring and dissolving is complete, and viscosity 1824mPa.s is to get aqueous labeling agent.
Embodiment 2
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:It is heated after 5g food-grades polyglutamic acid and 5g PEG-60 rilanit specials are mixed To 105-110 DEG C of insulated and stirred 5min, then 0-5 DEG C of heat preservation standing 1h is cooled to the cooling rate of 5 DEG C/min and is helped to get film forming Agent;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Embodiment 3
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:By 5g food-grades polyglutamic acid, 5g PEG-60 rilanit specials and 5g nanometre glues It is heated to 105-110 DEG C of insulated and stirred 5min after powder mixing, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and is stood 1h is to get coalescents;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
The preparation of nanometer rubber powder:1g Brazil waxs are added into 3g polyethylene glycol oxides, and are heated to molten condition heat preservation Stirring, adds 3g super fine magnesias, nanometer powder is made to get nanometre glue using nano-level grinder while hot after mixing Powder.
Embodiment 4
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:By 5g food-grades polyglutamic acid, 5g PEG-60 rilanit specials and 5g nanometre glues It is heated to 105-110 DEG C of insulated and stirred 5min after powder mixing, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and is stood 1h is to get coalescents;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
The preparation of nanometer rubber powder:2g Brazil waxs are added into 5g polyethylene glycol oxides, and are heated to molten condition heat preservation Stirring, adds 5g super fine magnesias, nanometer powder is made to get nanometre glue using nano-level grinder while hot after mixing Powder.
Reference examples 1
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:5g food-grade polyglutamic acids are heated to 105-110 DEG C of insulated and stirred 5min, then It is cooled to 0-5 DEG C of heat preservation with the cooling rate of 5 DEG C/min and stands 1h to get coalescents;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Reference examples 2
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:5g PEG-60 rilanit specials are heated to 105-110 DEG C of insulated and stirred 5min, then It is cooled to 0-5 DEG C of heat preservation with the cooling rate of 5 DEG C/min and stands 1h to get coalescents;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Reference examples 3
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) preparation of coalescents:It is heated after 5g food-grades polyglutamic acid and 5g PEG-60 rilanit specials are mixed To 105-110 DEG C of insulated and stirred 5min, then 0-5 DEG C of heat preservation standing 1h is cooled to the cooling rate of 5 DEG C/min and is helped to get film forming Agent;
(3) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g cetanols are added In water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Reference examples 4
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set 8g hydrolysis of polymaleic anhydride is added after rate 700W, reflow treatment 5min, stirs evenly, continues reflow treatment 10min, gained mixing Lotion is made through being concentrated under reduced pressure in object, and lotion is sent into after cooled to room temperature in freeze drier, and dry obtained solid is through powder Particle is made in broken machine;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of aqueous labeling agent:100g gelatin after pretreatment and 5g are modified cetanol to be added to the water, stirred Dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Reference examples 5
(1) pretreatment of gelatin:Will 100g edible gelatins be added 8 times of weight water in, be dispersed with stirring uniformly be placed on it is super In sound wave-microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave work(are set It being stirred evenly after rate 700W, reflow treatment 5min, continues reflow treatment 10min, lotion is made through being concentrated under reduced pressure in gained mixture, Lotion is sent into after cooled to room temperature in freeze drier, and particle is made through pulverizer in dry obtained solid;
(2) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(3) preparation of coalescents:It is heated after 5g food-grades polyglutamic acid and 5g PEG-60 rilanit specials are mixed To 105-110 DEG C of insulated and stirred 5min, then 0-5 DEG C of heat preservation standing 1h is cooled to the cooling rate of 5 DEG C/min and is helped to get film forming Agent;
(4) preparation of aqueous labeling agent:100g gelatin after pretreatment, 10g coalescents and 5g are modified cetanol It is added to the water, stirring and dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Reference examples 6
(1) chemical modification of cetanol:After 10g cetanols and 10g L-Glutimic acids are mixed plus absolute ethyl alcohol dissolves, The concentrated sulfuric acid is added dropwise again and adjusts solution ph to 4-5, and is heated to reflux state insulated and stirred, stops heating, warp after reaction Recycling ethyl alcohol is concentrated under reduced pressure, condensate residue is dissolved in water completely, and gained mixed liquor is sent into spray dryer, dry gained Micro mist is made to get modified cetanol through micronizer in grain;
(2) preparation of coalescents:It is heated after 5g food-grades polyglutamic acid and 5g PEG-60 rilanit specials are mixed To 105-110 DEG C of insulated and stirred 5min, then 0-5 DEG C of heat preservation standing 1h is cooled to the cooling rate of 5 DEG C/min and is helped to get film forming Agent;
(3) preparation of aqueous labeling agent:100g gelatin, 10g coalescents and 5g modification cetanol are added to the water, stirred Dissolving is complete, and viscosity 1759mPa.s is to get aqueous labeling agent.
Embodiment 5
Based on embodiment 2, be arranged do not added when prepared by coalescents PEG-60 rilanit specials reference examples 1, The reference examples 2 of food-grade polyglutamic acid are not added when prepared by coalescents, without the reference examples of cetanol chemical modification 3, do not add the reference examples 4 of coalescents, the reference examples 5 for not adding when gelatin pre-processes hydrolysis of polymaleic anhydride, without The pretreated reference examples of gelatin 6.
Be utilized respectively embodiment 1-4, reference examples 1-5 prepares aqueous labeling agent, and by made aqueous labeling agent be used for batch The label of same specification beer bottle is pasted, and the dosage of aqueous labeling agent is identical, and adhesive strength is measured after labeling agent is fully cured;Again The beer bottle for posting label is placed in 20-25 DEG C of water and impregnates 15min, observation label removes situation, and measures and pasted on beer bottle The clearance rate of agent is marked, the results are shown in Table 1.
The service condition of the aqueous labeling agent of 1 present invention of table
Group Adhesive strength/MPa Label removes situation Label agent clearance rate/%
Embodiment 1 3.8 Label completely strips 99.53
Embodiment 2 3.9 Label completely strips 99.61
Embodiment 3 4.3 Label completely strips 99.75
Embodiment 4 4.5 Label completely strips 99.84
Reference examples 1 3.7 Label completely strips 99.12
Reference examples 2 3.3 Label completely strips 98.37
Reference examples 3 2.7 Label is largely removed 96.59
Reference examples 4 1.9 Label is largely removed 93.26
Reference examples 5 1.5 Label fraction is removed 90.43
Reference examples 6 1.1 Label fraction is removed 87.15
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (7)

1. a kind of technique preparing aqueous labeling agent using ultrasonic-microwave collaboration method, which is characterized in that include the following steps:
(1) pretreatment of gelatin:Edible gelatin is added in the water of 5-10 times of weight, is dispersed with stirring and is uniformly placed on ultrasonic wave- In microwave synergistic extraction instrument, and supersonic frequency 40kHz, ultrasonic power 50W, microwave frequency 2450MHz, microwave power are set Hydrolysis of polymaleic anhydride is added after 700W, reflow treatment 5-10min, stirs evenly, continues reflow treatment 5-10min, gained is mixed It closes object and lotion is made through being concentrated under reduced pressure, lotion is sent into after cooled to room temperature in freeze drier, dry obtained solid warp Particle is made in pulverizer;
(2) chemical modification of cetanol:After cetanol and L-Glutimic acid are mixed plus absolute ethyl alcohol dissolves, then the concentrated sulfuric acid is added dropwise Solution ph is adjusted to 4-5, and is heated to reflux state insulated and stirred, stops heating after reaction, is recycled through being concentrated under reduced pressure Ethyl alcohol, condensate residue are dissolved in water completely, and gained mixed liquor is sent into spray dryer, and dry gained particle is through ultramicro grinding Micro mist is made to get modified cetanol in machine;
(3) preparation of coalescents:It is heated to 105-110 after food-grade polyglutamic acid and PEG-60 rilanit specials are mixed DEG C insulated and stirred 5-10min, then 0-5 DEG C of heat preservation is cooled to the cooling rate of 5 DEG C/min and stands 1-3h to get coalescents;
(4) preparation of aqueous labeling agent:Gelatin after pretreatment, coalescents and modified cetanol are added to the water, stirred Dissolving is complete, and viscosity control is in 1000-3000mPa.s to get aqueous labeling agent.
2. the technique according to claim 1 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:Edible gelatin in the step (1), hydrolysis of polymaleic anhydride mass ratio be 100:1-10.
3. the technique according to claim 1 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:Cetanol in the step (2), L-Glutimic acid mass ratio be 10:5-10.
4. the technique according to claim 1 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:Food-grade polyglutamic acid in the step (3), PEG-60 rilanit specials mass ratio be 5:1-5.
5. the technique according to claim 1 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:Gelatin after pretreatment in the step (4), coalescents, modified cetanol mass ratio be 100:5-15:1-10.
6. the technique according to claim 1 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:Coalescents also include the nanometer rubber powder with PEG-60 rilanit special equivalent, the preparation of nanometer rubber powder in the step (3) Method is:Brazil wax is added into polyethylene glycol oxide, and is heated to molten condition insulated and stirred, adds ultra-fine oxidation Nanometer powder is made to get nanometer rubber powder using nano-level grinder while hot after mixing in magnesium.
7. the technique according to claim 6 for being prepared aqueous labeling agent using ultrasonic-microwave collaboration method, feature are existed In:The polyethylene glycol oxide, Brazil wax, super fine magnesia mass ratio be 1-5:1-5:1-5.
CN201810423540.9A 2018-05-06 2018-05-06 Process for preparing water-based labeling agent by using ultrasonic-microwave synergistic method Active CN108624284B (en)

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CN105713545A (en) * 2016-03-30 2016-06-29 安徽青花坊瓷业股份有限公司 Adhesive for handles of ceramic cups
CN107201191A (en) * 2017-07-14 2017-09-26 许炳初 A kind of glass pack is packed for label paper adhesive

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CN105713545A (en) * 2016-03-30 2016-06-29 安徽青花坊瓷业股份有限公司 Adhesive for handles of ceramic cups
CN107201191A (en) * 2017-07-14 2017-09-26 许炳初 A kind of glass pack is packed for label paper adhesive

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