CN106700983A - Processing technique for glue - Google Patents

Processing technique for glue Download PDF

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Publication number
CN106700983A
CN106700983A CN201710011007.7A CN201710011007A CN106700983A CN 106700983 A CN106700983 A CN 106700983A CN 201710011007 A CN201710011007 A CN 201710011007A CN 106700983 A CN106700983 A CN 106700983A
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Prior art keywords
parts
glue
temperature
butyl
acetate
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CN201710011007.7A
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CN106700983B (en
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孙和平
章裕萍
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Kunming Heyu Adhesive Products Co Ltd
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Kunming Heyu Adhesive Products Co Ltd
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Priority to CN201710011007.7A priority Critical patent/CN106700983B/en
Priority to CN201810203989.4A priority patent/CN108329871B/en
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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
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/10Homopolymers or copolymers of methacrylic acid esters
    • 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
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/062Copolymers with monomers not covered by C09J133/06
    • C09J133/066Copolymers with monomers not covered by C09J133/06 containing -OH groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • 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
    • 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
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention belongs to the technical field of chemical engineering and aims at providing a processing technique with the advantages of little influence from temperature and humidity environments and good levelling property for glue. The processing technique for the glue is prepared from the following raw materials in parts by weight: 50 to 60 parts of methylbutyl acrylate, 3 to 6 parts of acrylic acid, 15 to 25 parts of butyl acetate, 8 to 12 parts of hydroxypropyl acrylate, 1 to 3 parts of oxazolidine, 4 to 6 parts of a silane coupling agent A-151, 15 to 20 parts of terpene resin, 3 to 8 parts of cellulose acetate butyrate, 4 to 6 parts of tert-butyl peroxybenzoate, 3 to 5 parts of benzoyl peroxide, 1 to 3 parts of zinc acetate, 20 to 30 parts of ethyl acetate, 72 to 78 parts of dimethylbenzene, 12 to 22 parts of dichloromethane and 10 to 20 parts of normal butanol. According to the processing technique disclosed by the invention, the toxicity of the glue is effectively reduced, the influence from the ambient temperature and humidity in a production process is little and the leveling property of the glue is remarkably enhanced; the glue can be produced in most areas.

Description

A kind of glue processing technology
Technical field
The invention belongs to chemical technology field, and in particular to glue processing technology.
Background technology
Glue includes water-base cement and oily gum, and water-base cement is by special using water as solvent by acrylic acid or polyurethane resin The emulsifying device of door, emulsification is formed, and this kind of glue is cheap, more environmental protection, but the film forming of water-base cement is poor, washing fastness Difference.Oily gum is based on oil-based solvent, acrylic acid or polyurethane dissolving to be formed, and this kind of glue good film-forming property, fastness are good, Using more universal, but this kind of glue feature of environmental protection difference, it is necessary to using some solvents with toxicity.In the prior art, it is enhancing The bonding force of glue, or some characteristic effects are reached, the reduction glue thickness such as on the premise of cohesive force is ensured needs more Using toxic solvents such as toluene, be so unfavorable for producing glue workman it is healthy, also result in glue production condition more Plus it is strict.
And oily gum is in process of production it is noted that avoid the incorporation of moisture, moisture can reduce the bonding effect of glue, especially It easily has moisture to be condensed in the equipment of glue in humid environment, the area of high humidity, will result in moisture and penetrates into glue In.Accordingly, it would be desirable to limit the humiture environment of production glue, to ensure the final product quality of glue, this is just proposed to power house environment Requirements at the higher level, increased production cost.Additionally, in the larger area of the temperature difference, the use of glue can also be affected, for example, Under low temperature environment, sticky, the levelability that glue can become decline so that glue is solidified into the shape of out-of-flatness, shadow in body surface Ring appearance.
The content of the invention
It is an object of the invention to provide a kind of by humiture ambient influnence is small, good leveling property glue processing technology.
For achieving the above object, the technical solution adopted in the present invention is:A kind of glue processing technology, raw material is by weight Gauge includes:
50~60 parts of butyl methacrylate, 3~6 parts of acrylic acid, 15~25 parts of butyl acetate, 8~12 parts of hydroxypropyl acrylate, 1~3 part of oxazolidine, 4~6 parts of silane coupling A -151,15~20 parts of terpene resin, 3~8 parts of acetylbutyrylcellulose, mistake 4~6 parts of t-butyl perbenzoate of oxidation, 3~5 parts of benzoyl peroxide, 1~3 part of zinc acetate, 20~30 parts of ethyl acetate, diformazan 72~78 parts of benzene, 12~22 parts of dichloromethane, 10~20 parts of n-butanol.
Preferably:Described raw material includes by weight:
55 parts of butyl methacrylate, 5 parts of acrylic acid, 20 parts of butyl acetate, 10 parts of hydroxypropyl acrylate, 2 parts of oxazolidine, silane 5 parts of coupling agent A-151,18 parts of terpene resin, 5 parts of acetylbutyrylcellulose, 5 parts of peroxidized t-butyl perbenzoate, benzoyl peroxide 4 parts of formyl, 2 parts of zinc acetate, 25 parts of ethyl acetate, 75 parts of dimethylbenzene, 18 parts of dichloromethane, 15 parts of n-butanol.
Preferably:Described acetylbutyrylcellulose uses CAB 381-20.
Preferably:Described glue processing technology is comprised the following steps:
1), the 80% of dimethylbenzene total amount is mixed with ethyl acetate, add butyl methacrylate and hydroxypropyl acrylate;Again will Acrylic acid mixes with the 50% of n-butanol total amount, and then both mix, and gradually heat up;It is 110r/ to control speed of agitator Min, programming rate is 3 DEG C/min, treats that temperature rises to 50~55 DEG C and stops heating up, and keeps the temperature to stir 30~50min.
2), first by the 60% of butyl acetate total amount and peroxidized t-butyl perbenzoate mix, be then slowly added into step 1)'s In reactant, speed of agitator 90r/min is maintained in adition process, then react 15~30min.
3), temperature is risen to 75~80 DEG C, then with remaining n-Butanol soluble benzoyl peroxide, and add reactant In, 80~110min is reacted, maintain speed of agitator 90r/min.
4), temperature is down to 40~45 DEG C, remaining dimethylbenzene and dichloromethane are mixed, for dissolving terpene resin; Acetylbutyrylcellulose is dissolved with remaining butyl acetate again, the terpene resin and acetylbutyrylcellulose after dissolving are added respectively Enter step 3)Reactant in, stir 55~80min, and stop heating, temperature is down to room temperature naturally;It is subsequently adding oxazole Alkane, silane coupling A -151 and zinc acetate, stirring are well mixed to each component, obtain final product.
Preferably:Described is slowly added to mode to be at the uniform velocity added dropwise, and rate of addition is 5ml/min.
Preferably:Described terpene resin is dissolved in the process of dimethylbenzene and dichloromethane mixture using ultrasonically treated, surpasses Acoustical power is 300~400W, and ultrasonic time is 5~10min.
The invention has the advantages that:Glue toxicity is effectively reduced, and ambient temperature and humidity shadow is received in production process Sound is small, can realize production in most of areas, hence it is evident that enhance the levelability of glue.Specifically, the present invention have adjusted glue The composition of water, using dimethylbenzene as solvent, each composition can well dissolve, be well mixed in making glue, and dimethylbenzene Toxicity is less than toluene, this reduces the toxicity using solvent, is conducive to improving the workshop condition of production glue, is also beneficial to Staff's is healthy, is easy to reduce the control to working condition.Meanwhile, added in the production technology that the present invention is provided Oxazolidine, the composition is extremely sensitive to water, and meeting very first time when moisture is run into decomposes, to remove the moisture being mixed into glue, Moisture is avoided to impact the cohesive force of glue.Accordingly even when in the larger area of humidity, it is not required that special configuration is controlled The equipment of workshop humidity, effectively reduces the production cost of glue, expands the scope that can be used as grown place.
Additionally, the not good phenomenon of levelability often occurs in use in glue, this can cause glue to solidify not in body surface Smooth phenomenon occurs, and outward appearance is had undesirable effect.And levelability it is not good the reason for, mainly too low with glue temperature, glue Caused by becoming sticky, and with glue temperature be on the one hand environment temperature influence, on the other hand also with the acetic acid second that contains in glue Ester is relevant.Ethyl acetate highly volatile, and this physical process of volatilizing can absorb heat, and cause glue temperature further to reduce, therefore The consumption of ethyl acetate is reduced in the present invention, and increased the amount of butyl acetate and n-butanol, to ensure each composition in glue Can well dissolve, mix.And acetylbutyrylcellulose is added in the present invention, the composition can improve the levelling of glue Property, the cohesive force without influenceing glue.
Specific embodiment
Lower mask body provides preferred embodiment so that those skilled in the art more understand technical scheme and Effect.
Embodiment one
1), by weight, 60 parts of dimethylbenzene are mixed with 25 parts of ethyl acetate, in mixture add 55 parts of methacrylic acid fourths Ester and 10 parts of hydroxypropyl acrylates;5 parts of acrylic acid are mixed with 7.5 parts of n-butanols again, then both mix, and gradually rise Temperature.That is, the butyl methacrylate and hydroxypropyl acrylate of dimethylbenzene and ethyl acetate will be dissolved in and n-butanol is dissolved in Acrylic acid mixing.Control speed of agitator for 110r/min, programming rate is 3 DEG C/min, treats that temperature rises to 50~55 DEG C of stoppings Heat up, keep the temperature to stir 40min.By by butyl methacrylate, hydroxypropyl acrylate and acrylic acid respectively with accordingly Solvent mixes, then the stirring that heats up, and is conducive to these three compositions preferably to disperse in mixed solvent, makes its reaction more thorough.
2), first 12 parts of butyl acetates and 5 parts of peroxidized t-butyl perbenzoates are mixed, be then slowly added into step 1)It is anti- Answer in thing, speed of agitator 90r/min is maintained in adition process, then react 25min.Being slowly added to here can be using can The feeder of liquid feeding speed is controlled, is at the uniform velocity added dropwise, it is 5ml/min to control rate of addition.
3), temperature is risen to 75~80 DEG C, then with 7.5 parts of n-Butanol solubles, 4 parts of benzoyl peroxides, and add reaction In thing, 95min is reacted, maintain speed of agitator 90r/min.Reactant further reacts in stirring, temperature higher and slower Mixing speed be conducive to reaction carrying out.
4), temperature is down to 40~45 DEG C, 15 parts of dimethylbenzene and 18 parts of dichloromethane are mixed, for dissolving 18 parts of terpenes Resin;5 parts of CAB 381-20 are dissolved with 8 parts of butyl acetates again, the terpene resin after dissolving and acetylbutyrylcellulose are distinguished Add step 3)Reactant in, stir 70min, and stop heating, temperature is down to room temperature naturally.Because terpene resin is two Solubility in chloromethanes is better than the solubility in dimethylbenzene, and dichloromethane has volatility, two as ethyl acetate The content of chloromethanes is larger to be easily caused glue temperature is relatively low and influence levelability when in use, therefore uses dimethylbenzene and dichloromethane The mixture of alkane dissolves terpene resin.If terpene resin is difficult to quick dissolving, can be to terpene resin and dimethylbenzene and dichloro The mixture of methane carries out ultrasonically treated, and ultrasonic power is 350W, and ultrasonic time is 8min.Be eventually adding 2 parts of oxazolidines, 5 parts Silane coupling A -151 and 2 parts of zinc acetates, stirring are well mixed to each component, obtain final product.
Embodiment two
1), by weight, 62 parts of dimethylbenzene are mixed with 26 parts of ethyl acetate, in mixture add 56 parts of methacrylic acid fourths Ester and 11 parts of hydroxypropyl acrylates;5 parts of acrylic acid are mixed with 8 parts of n-butanols again, then both mix, and gradually rise Temperature.Control speed of agitator for 110r/min, programming rate is 3 DEG C/min, treat that temperature rises to 50~55 DEG C and stops heating up, keeping should Temperature stirs 43min.
2), first 13.2 parts of butyl acetates and 5 parts of peroxidized t-butyl perbenzoates are mixed, be then slowly added into step 1)'s In reactant, speed of agitator 90r/min is maintained in adition process, then react 23min.Being slowly added to here can use energy The feeder of liquid feeding speed is enough controlled, is at the uniform velocity added dropwise, it is 5ml/min to control rate of addition.
3), temperature is risen to 75~80 DEG C, then with 8 parts of n-Butanol solubles, 4 parts of benzoyl peroxides, and add reactant In, 100min is reacted, maintain speed of agitator 90r/min.
4), temperature is down to 40~45 DEG C, 15.5 parts of dimethylbenzene and 17 parts of dichloromethane are mixed, for dissolving 17 parts of terpenes Olefine resin;6 parts of CAB 381-20 are dissolved with 8.8 parts of butyl acetates again, by terpene resin and acetylbutyrylcellulose after dissolving It is separately added into step 3)Reactant in, stir 65min, and stop heating, temperature is down to room temperature naturally.If terpene resin Quick dissolving is difficult to, terpene resin and the mixture of dimethylbenzene and dichloromethane can be carried out ultrasonically treated, ultrasonic power is 350W, ultrasonic time is 7min.2.2 parts of oxazolidines, 5 parts of silane coupling As -151 and 2.1 parts of zinc acetates are eventually adding, are stirred It is well mixed to each component, obtain final product.
Embodiment three
1), by weight, 57.6 parts of dimethylbenzene are mixed with 20 parts of ethyl acetate, in mixture add 50 parts of methacrylic acids Butyl ester and 8 parts of hydroxypropyl acrylates;3 parts of acrylic acid are mixed with 5 parts of n-butanols again, then both mix, and gradually rise Temperature.Control speed of agitator for 110r/min, programming rate is 3 DEG C/min, treat that temperature rises to 50~55 DEG C and stops heating up, keeping should Temperature stirs 30min.
2), first 9 parts of butyl acetates and 4 parts of peroxidized t-butyl perbenzoates are mixed, be then slowly added into step 1)It is anti- Answer in thing, speed of agitator 90r/min is maintained in adition process, then react 15min.Being slowly added to here can be using can The feeder of liquid feeding speed is controlled, is at the uniform velocity added dropwise, it is 5ml/min to control rate of addition.
3), temperature is risen to 75~80 DEG C, then with 5 parts of n-Butanol solubles, 3 parts of benzoyl peroxides, and add reactant In, 80min is reacted, maintain speed of agitator 90r/min.
4), temperature is down to 40~45 DEG C, 14.4 parts of dimethylbenzene and 12 parts of dichloromethane are mixed, for dissolving 15 parts of terpenes Olefine resin;3 parts of CAB 381-20 are dissolved with 6 parts of butyl acetates again, by the terpene resin and acetylbutyrylcellulose after dissolving point Jia Ru not step 3)Reactant in, stir 55min, and stop heating, temperature is down to room temperature naturally.If terpene resin is difficult Quickly to dissolve, terpene resin and the mixture of dimethylbenzene and dichloromethane can be carried out ultrasonically treated, ultrasonic power is 400W, Ultrasonic time is 5min.1 part of oxazolidine, 4 parts of silane coupling As -151 and 1 part of zinc acetate are eventually adding, stirring is mixed to each component Close uniform, obtain final product.
Example IV
1), by weight, 62.4 parts of dimethylbenzene are mixed with 30 parts of ethyl acetate, in mixture add 60 parts of methacrylic acids Butyl ester and 12 parts of hydroxypropyl acrylates;6 parts of acrylic acid are mixed with 10 parts of n-butanols again, then both mix, and gradually Heat up.Control speed of agitator for 110r/min, programming rate is 3 DEG C/min, treat that temperature rises to 50~55 DEG C and stops heating up, keep The temperature stirs 50min.
2), 15 parts of butyl acetates and 6 parts of peroxidized t-butyl perbenzoates are mixed, be slowly added to step 1)Reactant In, speed of agitator 90r/min is maintained in adition process, then react 30min.
3), temperature is risen to 75~80 DEG C, then with 10 parts of n-Butanol solubles, 5 parts of benzoyl peroxides, and add reaction In thing, 110min is reacted, maintain speed of agitator 90r/min.
4), temperature is down to 40~45 DEG C, 15.6 parts of dimethylbenzene and 22 parts of dichloromethane are mixed, for dissolving 20 parts of terpenes Olefine resin;8 parts of CAB 381-20 are dissolved with 10 parts of butyl acetates again, by the terpene resin and acetylbutyrylcellulose after dissolving point Jia Ru not step 3)Reactant in, stir 80min, and stop heating, temperature is down to room temperature naturally.It is eventually adding 3 parts of evils Oxazolidine, 6 parts of silane coupling As -151 and 3 parts of zinc acetates, stirring are well mixed to each component, obtain final product.
Comparative example one
Glue production is now carried out according to prior art, product glue is obtained as a comparison case.
1), by weight, by 35 parts of butyl acrylates, 10 parts of 2-EHAs, 0.5 part of acrylic acid, 1 part of propylene Sour hydroxyl ethyl ester, 30 parts of ethyl acetate and 60 parts of toluene are fitted into three neck round bottom, then three neck round bottom is connected respectively stir Device, thermometer and condenser are mixed, and the raw material added by the above is stirred by agitator, while will be former above by water-bath Material heating.
2), to be heated to 85 DEG C, while stirring add 0.3 part of benzoyl peroxide.
3), after the benzoyl peroxide temperature that is added is raised, maintain 85 DEG C of reaction 1h, add 0.5 part of peroxidating Benzoyl and 4 parts of ethyl acetate, continue to react.
4), after reaction 0.5h, add the double lauroyl of 2 parts of peroxidating and 5 parts of vinylacetates, and lower the temperature again after constant temperature 2h.
5), after room temperature is cooled to, add 10 parts of terpene phenol resins, 0.3 part of aluminium acetylacetonate, mix to each component It is well mixed, obtain final product.
Product checking
Further to verify beneficial effects of the present invention, respectively under normal humidity environment(Medial humidity 55%)And wet environment Under(Medial humidity 85%)The embodiment one to four of production and the product of comparative example one are detected.Detection content include viscosity, PH value, 23 DEG C of shear strengths, 70 DEG C of shear strengths, levelability, heat resistance and cold resistance.Detection method is as follows:
Viscosity:(23±2℃)Under the conditions of, determine the product of embodiment one to four and comparative example one respectively with rotational viscometer.
PH value:(23±2℃)Under the conditions of, embodiment one to four is determined respectively with the Numerical pH-meter of precision≤0.1 With the product of comparative example one.
23 DEG C of shear strengths:(23 ± 2 DEG C, humidity 45%~55%)Under the conditions of, respectively with embodiment one to four and contrast The product of example one is glued the same metal sheet of surfacing, is made sample.With the length of gage measuring sample faying surface And width, it is accurate to 0.05mm;Sample is symmetrically clipped in upper and lower holder, the distance of holding position to bond end is(50± 1)mm;Testing machine is started,(5±1)In mm/min, loaded with stabilized speed, record the peak load of sample failure by shear, meter Calculate shear strength.The computing formula of shear strength τ is as follows:
(F is failure by shear peak load;B and l are respectively that faying surface is wide, length)
70 DEG C of shear strengths:(70 ± 2 DEG C, humidity 45%~55%)Under the conditions of detected, detection method is strong with 23 DEG C of shearings Degree.
Levelability:(23 ± 2 DEG C, humidity 45%~55%)Under the conditions of, by embodiment one to four and the product of comparative example one On a glass, coating duration is not more than 20s for coating, determines glue surface and reaches uniform, smooth, wrinkle-free state required time.
Heat resistance:The product 100ml for distinguishing Example one to four and comparative example one with graduated cylinder moves into 250ml tool plug tapers In bottle, sealed after cleaning bottleneck, in temperature(50±2)Continue 5h under the conditions of DEG C, visually inspected immediately after taking-up, glue is without knot The significant changes such as block, layering are qualified.
Cold resistance:The product of embodiment one to four and comparative example one to test tube is added in having ground glass stopper test tube respectively 1/3rd at, clean it is closed after bottleneck, in temperature(-15±3)Under the conditions of DEG C, continue 5h, treated after taking-up glue recover to Normal temperature(20±15)DEG C, after being stirred with glass bar, put upside down and just put each 3 times.Visually inspect, glue without caking, mobility without Significant change is qualified.
Obtain testing result as shown in the table:
Product checking result is produced under the normal humidity environment of table 1
Project Embodiment one Embodiment two Embodiment three Example IV Comparative example one
Viscosity(Pa·s) 3.6 3.7 3.5 3.8 2.8
PH value 6.5 6.5 6.4 6.5 6.8
23 DEG C of shear strengths(MPa) 30 31 29 28 26
70 DEG C of shear strengths(MPa) 31 30 22 23 15
Levelability(s) 42 45 48 36 It is unable to reach levelling state
Heat resistance It is qualified It is qualified It is qualified It is qualified It is qualified
Cold resistance It is qualified It is qualified It is qualified It is qualified It is qualified
Product checking result is produced under the wet environment of table 2
Project Embodiment one Embodiment two Embodiment three Example IV Comparative example one
Viscosity(Pa·s) 3.2 3.3 3.1 3.5 0.9
PH value 6.7 6.7 6.5 6.6 6.3
23 DEG C of shear strengths(MPa) 28 28 27 26 19
70 DEG C of shear strengths(MPa) 30 27 20 19 10
Levelability(s) 45 47 43 38 It is unable to reach levelling state
Heat resistance It is qualified It is qualified It is qualified It is qualified It is qualified
Cold resistance It is qualified It is qualified It is qualified It is qualified It is qualified
Understood with reference to Tables 1 and 2, the glue bonding effect of present invention production is good, the product for either being produced under normal humidity environment The product produced under product or wet environment, the shear strength for detecting at nominal room temperature and under the conditions of 70 DEG C is all higher than existing skill Art level.The present invention is hardly influenceed by ambient humidity, and the product viscosity for producing in wet condition is good, outclass existing skill The product that art is produced in wet condition.And compared to prior art, present invention improves the levelability of product, using Cheng Zhong, ensure that pasted material, especially relatively thin material appearance is smooth, attractive in appearance, it is to avoid prior art production Glue is frozen into the phenomenon of roughness in body surface.

Claims (6)

1. a kind of glue processing technology, it is characterised in that:Raw material includes by weight:
50~60 parts of butyl methacrylate, 3~6 parts of acrylic acid, 15~25 parts of butyl acetate, 8~12 parts of hydroxypropyl acrylate, 1~3 part of oxazolidine, 4~6 parts of silane coupling A -151,15~20 parts of terpene resin, 3~8 parts of acetylbutyrylcellulose, mistake 4~6 parts of t-butyl perbenzoate of oxidation, 3~5 parts of benzoyl peroxide, 1~3 part of zinc acetate, 20~30 parts of ethyl acetate, diformazan 72~78 parts of benzene, 12~22 parts of dichloromethane, 10~20 parts of n-butanol.
2. glue processing technology according to claim 1, it is characterised in that:Described raw material includes by weight:
55 parts of butyl methacrylate, 5 parts of acrylic acid, 20 parts of butyl acetate, 10 parts of hydroxypropyl acrylate, 2 parts of oxazolidine, silane 5 parts of coupling agent A-151,18 parts of terpene resin, 5 parts of acetylbutyrylcellulose, 5 parts of peroxidized t-butyl perbenzoate, benzoyl peroxide 4 parts of formyl, 2 parts of zinc acetate, 25 parts of ethyl acetate, 75 parts of dimethylbenzene, 18 parts of dichloromethane, 15 parts of n-butanol.
3. glue processing technology according to claim 1, it is characterised in that:Described acetylbutyrylcellulose uses CAB 381-20。
4. glue processing technology according to claim 1 and 2, it is characterised in that:Described glue processing technology include with Lower step:
1), the 80% of dimethylbenzene total amount is mixed with ethyl acetate, add butyl methacrylate and hydroxypropyl acrylate;Again will Acrylic acid mixes with the 50% of n-butanol total amount, and then both mix, and gradually heat up;It is 110r/ to control speed of agitator Min, programming rate is 3 DEG C/min, treats that temperature rises to 50~55 DEG C and stops heating up, and keeps the temperature to stir 30~50min;
2), first by the 60% of butyl acetate total amount and peroxidized t-butyl perbenzoate mix, be then slowly added into step 1)Reaction In thing, speed of agitator 90r/min is maintained in adition process, then react 15~30min;
3), temperature is risen to 75~80 DEG C, then with remaining n-Butanol soluble benzoyl peroxide, and add reactant, 80~110min of reaction, maintains speed of agitator 90r/min;
4), temperature is down to 40~45 DEG C, remaining dimethylbenzene and dichloromethane are mixed, for dissolving terpene resin;Use again Remaining butyl acetate dissolves acetylbutyrylcellulose, and the terpene resin and acetylbutyrylcellulose after dissolving are separately added into step Rapid 3)Reactant in, stir 55~80min, and stop heating, temperature is down to room temperature naturally;It is subsequently adding oxazolidine, silicon Alkane coupling agent A-151 and zinc acetate, stirring are well mixed to each component, obtain final product.
5. glue processing technology according to claim 4, it is characterised in that:Described is slowly added to mode at the uniform velocity to drip Plus, rate of addition is 5ml/min.
6. glue processing technology according to claim 4, it is characterised in that:Described terpene resin is dissolved in dimethylbenzene and two The process of chloromethane mixture uses ultrasonically treated, and ultrasonic power is 300~400W, and ultrasonic time is 5~10min.
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