CN106700983B - A kind of glue processing technology - Google Patents
A kind of glue processing technology Download PDFInfo
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- CN106700983B CN106700983B CN201710011007.7A CN201710011007A CN106700983B CN 106700983 B CN106700983 B CN 106700983B CN 201710011007 A CN201710011007 A CN 201710011007A CN 106700983 B CN106700983 B CN 106700983B
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- 239000003292 glue Substances 0.000 title claims abstract description 59
- 238000005516 engineering process Methods 0.000 title claims abstract description 14
- 238000012545 processing Methods 0.000 title claims abstract description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 51
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 51
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 150000003505 terpenes Chemical class 0.000 claims abstract description 28
- 235000007586 terpenes Nutrition 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims abstract description 18
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 16
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims abstract description 13
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 12
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 10
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000077 silane Inorganic materials 0.000 claims abstract description 10
- WYNCHZVNFNFDNH-UHFFFAOYSA-N Oxazolidine Chemical compound C1COCN1 WYNCHZVNFNFDNH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000008878 coupling Effects 0.000 claims abstract description 9
- 238000010168 coupling process Methods 0.000 claims abstract description 9
- 238000005859 coupling reaction Methods 0.000 claims abstract description 9
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 8
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004246 zinc acetate Substances 0.000 claims abstract description 8
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000376 reactant Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 239000007822 coupling agent Substances 0.000 claims 2
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 231100000419 toxicity Toxicity 0.000 abstract description 5
- 230000001988 toxicity Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 12
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 235000013904 zinc acetate Nutrition 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 150000002917 oxazolidines Chemical class 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- KILURZWTCGSYRE-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]alumanyloxypent-3-en-2-one Chemical compound CC(=O)\C=C(\C)O[Al](O\C(C)=C/C(C)=O)O\C(C)=C/C(C)=O KILURZWTCGSYRE-LNTINUHCSA-K 0.000 description 1
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- PVEOYINWKBTPIZ-UHFFFAOYSA-N but-3-enoic acid Chemical class OC(=O)CC=C PVEOYINWKBTPIZ-UHFFFAOYSA-N 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical class CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- -1 hydroxyl ethyl Chemical group 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 125000000400 lauroyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives 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
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives 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
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- 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 chemical technology fields.Purpose is to provide a kind of is influenced small, good leveling property glue processing technology by humiture environment.The raw material of the glue processing technology 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, 151 4~6 parts of silane coupling A, 15~20 parts of terpene resin, 3~8 parts of acetylbutyrylcellulose, 4~6 parts of peroxidized t-butyl perbenzoate, 3~5 parts of benzoyl peroxide, 1~3 part of zinc acetate, 20~30 parts of ethyl acetate, 72~78 parts of dimethylbenzene, 12~22 parts of dichloromethane, 10~20 parts of n-butanol.The present invention effectively reduces glue toxicity, and is influenced by ambient temperature and humidity small in production process, can realize production in most of areas, hence it is evident that enhance the levelability of glue.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to glue processing technology.
Background technology
Glue include water-base cement and oily gum, water-base cement be acrylic acid or polyurethane resin are passed through using water as solvent it is special
The emulsifying device of door, emulsifies, and this kind of glue is cheap, more environmentally friendly, but the film forming of water-base cement is poor, washing fastness
Difference.Oily gum is based on oil-based solvent, and acrylic acid or polyurethane are dissolved, and this kind of glue good film-forming property, fastness are good,
Using more universal, but the feature of environmental protection difference of this kind of glue is, it is necessary to using some solvents with toxicity.In the prior art, it is enhancing
The bonding force of glue reaches some characteristic effects, such as the reduction glue thickness on the premise of cohesive force is ensured, needs more
Using toxic solvents such as toluene, so it is unfavorable for producing the health of the worker of glue, also results in glue production condition more
Add stringent.
And oily gum, in process of production it is noted that avoiding 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 the big area of humid environment, humidity, will result in moisture and penetrates into glue
In.Therefore, it is necessary to limit the humiture environment of production glue, to ensure the final product quality of glue, this just proposes power house environment
Requirements at the higher level add production cost.In addition, in the larger area of the temperature difference, the use of glue can also be affected, for example,
Under low temperature environment, sticky, 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
The object of the present invention is to provide a kind of small, good leveling property glue processing technology is influenced by humiture environment.
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, hydroxypropyl acrylate 8~
12 parts, 1~3 part of oxazolidine, 4~6 parts of silane coupling A -151,15~20 parts of terpene resin, acetylbutyrylcellulose 3~8
Part, 4~6 parts of peroxidized t-butyl perbenzoate, 3~5 parts of benzoyl peroxide, 1~3 part of zinc acetate, 20~30 parts of ethyl acetate,
72~78 parts of dimethylbenzene, 12~22 parts of dichloromethane, 10~20 parts of n-butanol.
Preferably：The 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,
5 parts of silane coupling A -151,18 parts of terpene resin, 5 parts of acetylbutyrylcellulose, 5 parts of peroxidized t-butyl perbenzoate, peroxide
Change 4 parts of benzoyl, 2 parts of zinc acetate, 25 parts of ethyl acetate, 75 parts of dimethylbenzene, 18 parts of dichloromethane, 15 parts of n-butanol.
Preferably：The acetylbutyrylcellulose uses CAB 381-20.
Preferably：The glue processing technology comprises the following steps：
1）, the 80% of dimethylbenzene total amount is mixed with ethyl acetate, add in butyl methacrylate and hydroxypropyl acrylate；
Acrylic acid is mixed with the 50% of n-butanol total amount again, then the two is mixed, and gradually heats up；The speed of agitator is controlled to be
110r/min, heating rate be 3 DEG C/min, treat temperature rise to 50~55 DEG C stop heating, keep the temperature stirring 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 reacts 15~30min.
3）, temperature is risen to 75~80 DEG C, then with remaining n-Butanol soluble benzoyl peroxide, and add in reactant
In, 80~110min is reacted, maintains speed of agitator 90r/min.
4）, temperature is made to be down to 40~45 DEG C, remaining dimethylbenzene and dichloromethane are mixed, for dissolving terpene resin；
Acetylbutyrylcellulose is dissolved with remaining butyl acetate again, dissolved terpene resin and acetylbutyrylcellulose are added respectively
Enter step 3）Reactant in, stir 55~80min, and stop heating, temperature is made to be down to room temperature naturally；Then oxazole is added in
Alkane, silane coupling A -151 and zinc acetate, stir to each component be uniformly mixed to get.
Preferably：Described is slowly added to mode to be at the uniform velocity added dropwise, rate of addition 5ml/min.
Preferably：The terpene resin is dissolved in the process of dimethylbenzene and dichloromethane mixture using being ultrasonically treated, and surpasses
Acoustical power is 300~400W, and ultrasonic time is 5~10min.
The invention has the advantages that：Glue toxicity is effectively reduced, and by ambient temperature and humidity shadow 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 has adjusted glue
The ingredient of water using dimethylbenzene as solvent, makes each ingredient in glue that can dissolve, be uniformly mixed well, and dimethylbenzene
Toxicity is less than toluene, and this reduces the toxicity for using solvent, are conducive to improve the workshop condition of production glue, are also beneficial to
The health of staff, convenient for reducing the control to working condition.Meanwhile it is added in production technology provided by the invention
Oxazolidine, the ingredient is extremely sensitive to water, can at the first time be decomposed when running into moisture, 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 controls
The equipment of workshop humidity effectively reduces the production cost of glue, expands the scope that can be used as grown place.
In addition, the phenomenon that levelability is bad often occurs in use in glue, this can cause glue to cure not in body surface
The phenomenon that smooth, occurs, and harmful effect is caused to appearance.And levelability it is bad the reason for, mainly too low with glue temperature, glue
Caused by becoming sticky, and with glue temperature be on the one hand the influence of environment temperature, on the other hand also with the acetic acid second that contains in glue
Ester is related.Ethyl acetate highly volatile, and this physical process of volatilizing can absorb heat, and glue temperature is caused further to reduce, therefore
Reduce the dosage of ethyl acetate in the present invention, and add the amount of butyl acetate and n-butanol, to ensure each ingredient in glue
It can dissolve, mix well.And acetylbutyrylcellulose is added in the present invention, which can improve the levelling of glue
Property, the cohesive force without influencing 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, into mixture add in 55 parts of metering systems
Acid butyl ester and 10 parts of hydroxypropyl acrylates；5 parts of acrylic acid are mixed with 7.5 parts of n-butanols again, then the two is mixed, and by
Edge up temperature.That is, it by the butyl methacrylate for being dissolved in dimethylbenzene and ethyl acetate and hydroxypropyl acrylate and is dissolved in just
The acrylic acid mixing of butanol.Controlling speed of agitator, heating rate is 3 DEG C/min, treats that temperature rises to 50~55 DEG C for 110r/min
Stop heating, the temperature is kept to stir 40min.By by butyl methacrylate, hydroxypropyl acrylate and acrylic acid respectively with
Coordinative solvent mixes, then the stirring that heats up, and is conducive to these three ingredients and is better dispersed in the mixed solvent, makes its reaction more thorough
Bottom.
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-
It answers in object, speed of agitator 90r/min is maintained in adition process, then reacts 25min.Here be slowly added to may be employed 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 in reaction
In object, 95min is reacted, maintains speed of agitator 90r/min.Reactant further reacts in stirring, higher temperature and relatively slow
Mixing speed be conducive to reaction progress.
4）, temperature is made to be 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, dissolved terpene resin and acetylbutyrylcellulose are distinguished
Add in step 3）Reactant in, stir 70min, and stop heating, temperature is made to be down to room temperature naturally.Since terpene resin is two
Solubility in chloromethanes better than the solubility in dimethylbenzene, and dichloromethane with ethyl acetate as with volatility, two
The content of chloromethanes is larger to be easy to cause glue temperature is relatively low and influence levelability when in use, therefore uses dimethylbenzene and dichloromethane
The mixture of alkane dissolves terpene resin.It, can be to terpene resin and dimethylbenzene and dichloro if terpene resin is difficult to quickly dissolve
The mixture of methane is ultrasonically treated, ultrasonic power 350W, ultrasonic time 8min.Be eventually adding 2 parts of oxazolidines, 5 parts
Silane coupling A -151 and 2 parts of zinc acetates, stir to each component be uniformly mixed to get.
Embodiment two
1）, by weight, 62 parts of dimethylbenzene are mixed with 26 parts of ethyl acetate, into mixture add in 56 parts of metering systems
Acid butyl ester and 11 parts of hydroxypropyl acrylates；5 parts of acrylic acid are mixed with 8 parts of n-butanols again, then the two is mixed, and gradually
Heating.Controlling speed of agitator, heating rate is 3 DEG C/min for 110r/min, treats that temperature rises to 50~55 DEG C and stops heating, keeps
The 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 reacts 23min.Energy may be employed in being slowly added to here
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 in reactant
In, 100min is reacted, maintains speed of agitator 90r/min.
4）, temperature is made to be 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 dissolved terpene resin and acetylbutyrylcellulose
It is separately added into step 3）Reactant in, stir 65min, and stop heating, temperature is made to be down to room temperature naturally.If terpene resin
It is difficult to quickly dissolve, the mixture of terpene resin and dimethylbenzene and dichloromethane can be ultrasonically treated, ultrasonic power is
350W, ultrasonic time 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
To each component be uniformly mixed to get.
Embodiment three
1）, by weight, 57.6 parts of dimethylbenzene are mixed with 20 parts of ethyl acetate, into mixture add in 50 parts of methyl-props
Olefin(e) acid butyl ester and 8 parts of hydroxypropyl acrylates；3 parts of acrylic acid are mixed with 5 parts of n-butanols again, then the two is mixed, and by
Edge up temperature.Controlling speed of agitator, heating rate is 3 DEG C/min for 110r/min, treats that temperature rises to 50~55 DEG C and stops heating, protects
Hold temperature stirring 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-
It answers in object, speed of agitator 90r/min is maintained in adition process, then reacts 15min.Here be slowly added to may be employed 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 in reactant
In, 80min is reacted, maintains speed of agitator 90r/min.
4）, temperature is made to be 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 dissolved terpene resin and acetylbutyrylcellulose point
It Jia Ru not step 3）Reactant in, stir 55min, and stop heating, temperature is made to be down to room temperature naturally.If terpene resin is difficult
Quickly to dissolve, the mixture of terpene resin and dimethylbenzene and dichloromethane can be ultrasonically treated, ultrasonic power 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, stirs to each component and mixes
Close uniformly to get.
Example IV
1）, by weight, 62.4 parts of dimethylbenzene are mixed with 30 parts of ethyl acetate, into mixture add in 60 parts of methyl-props
Olefin(e) acid butyl ester and 12 parts of hydroxypropyl acrylates；6 parts of acrylic acid are mixed with 10 parts of n-butanols again, then the two is mixed, and
Gradually heating.Controlling speed of agitator, heating rate is 3 DEG C/min for 110r/min, treats that temperature rises to 50~55 DEG C and stops heating,
The temperature is kept to stir 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 reacts 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 in reaction
In object, 110min is reacted, maintains speed of agitator 90r/min.
4）, temperature is made to be 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 dissolved terpene resin and acetylbutyrylcellulose point
It Jia Ru not step 3）Reactant in, stir 80min, and stop heating, temperature is made to be 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, stir to each component be uniformly mixed to get.
Comparative example one
Glue production is now carried out according to the prior art, obtains product glue 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 and is stirred
Device, thermometer and condenser are mixed, and passes through blender and stirs evenly above added raw material, while will be above former by water-bath
Material heating.
2）, to be heated to 85 DEG C, while stirring add in 0.3 part of benzoyl peroxide.
3）, wait added in benzoyl peroxide temperature rise after, maintain 85 DEG C reaction 1h, add 0.5 part of peroxidating
Benzoyl and 4 parts of ethyl acetate, the reaction was continued.
4）, after reaction 0.5h, add in the double lauroyl of 2 parts of peroxidating and 5 parts of vinylacetates, and cool down again after constant temperature 2h.
5）, after room temperature is cooled to, add in 10 parts of terpene phenol resins, 0.3 part of aluminium acetylacetonate, mix to each component
Be uniformly mixed to get.
Product testing
Further to verify beneficial effects of the present invention, respectively under normal humidity environment（Medial humidity 55%）And humidity
Under environment（Medial humidity 85%）The embodiment one to four of production and the product of comparative example one are detected.Detection content includes
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, measure the production of embodiment one to four and comparative example one respectively with rotational viscometer
Product.
PH value：（23±2℃）Under the conditions of, embodiment one to four is measured 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 comparison
The product of example one is glued the same metal sheet of surfacing, and sample is made.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）It in mm/min, is loaded with stabilized speed, records the peak load of sample failure by shear, meter
Calculate shear strength.The calculation formula of shear strength τ is as follows：
（F is failure by shear peak load；B and l is respectively that faying surface is wide, length）
70 DEG C of shear strengths：（70 ± 2 DEG C, humidity 45%~55%）Under the conditions of be detected, detection method is cut with 23 DEG C
Shearing stress.
Levelability：（23 ± 2 DEG C, humidity 45%~55%）Under the conditions of, by the product of embodiment one to four and comparative example one
On a glass, coating duration is not more than 20s for coating, measures glue surface and reaches uniform, smooth, wrinkle-free state required time.
Heat resistance：The product 100ml that Example one to four and comparative example one are distinguished 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 qualification.
Cold resistance：The product of embodiment one to four and comparative example one is added in having ground glass stopper test tube respectively to test tube
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
Room temperature（20±15）DEG C, after being stirred evenly with glass bar, put upside down and just put each 3 times.Visually inspect, glue without caking, mobility without
Significant change is qualification.
It is as shown in the table to obtain testing result：
Product testing result is produced under 1 normal humidity environment of table
| 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 testing result is produced under 2 wet environment of table
| 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 |
According to Tables 1 and 2, glue bonding effect produced by the invention is good, is either produced under normal humidity environment
Product or wet environment under the product that produces, the shear strength detected at nominal room temperature and under the conditions of 70 DEG C is all higher than existing
There is technical merit.The present invention is hardly influenced by ambient humidity, and the product viscosity produced in wet condition is good, outclass existing
There is the product that technology produces in wet condition.And compared with the prior art, make present invention improves the levelability of product
With that in the process, can ensure pasted material, especially relatively thin material appearance is smooth, beautiful, avoids prior art life
The glue of production is body surface is frozen into roughness the phenomenon that.
Claims (6)
1. a kind of glue, 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
Aoxidize 4~6 parts of t-butyl perbenzoate, 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 according to claim 1, it is characterised in that：The 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 according to claim 1, it is characterised in that：The acetylbutyrylcellulose uses CAB 381-20.
4. glue according to claim 1 or 2, it is characterised in that：The processing technology of the glue comprises the following steps：
1), the 80% of dimethylbenzene total amount with ethyl acetate is mixed, adds in butyl methacrylate and hydroxypropyl acrylate；Again will
Acrylic acid is mixed with the 50% of n-butanol total amount, and then the two is mixed, and gradually heats up；It is 110r/ to control speed of agitator
Min, heating rate are 3 DEG C/min, treat that temperature rises to 50~55 DEG C and stops heating, the temperature is kept to stir 30~50min；
2), first the 60% of butyl acetate total amount and peroxidized t-butyl perbenzoate are mixed, are then slowly added into the anti-of step 1)
It answers in object, 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 is added in reactant,
80~110min is reacted, maintains speed of agitator 90r/min；
4) temperature, is made to be down to 40~45 DEG C, remaining dimethylbenzene and dichloromethane are mixed, for dissolving terpene resin；It uses again
Remaining butyl acetate dissolves acetylbutyrylcellulose, and dissolved terpene resin and acetylbutyrylcellulose are separately added into step
In rapid reactant 3), 55~80min is stirred, and stops heating, temperature is made to be down to room temperature naturally；Then oxazolidine, silicon are added in
Alkane coupling agent A-151 and zinc acetate, stir to each component be uniformly mixed to get.
5. glue according to claim 4, it is characterised in that：Described is slowly added to mode to be at the uniform velocity added dropwise, and speed is added dropwise
It spends for 5ml/min.
6. glue according to claim 4, it is characterised in that：The terpene resin is dissolved in dimethylbenzene and dichloromethane mixes
The process of object is closed using being ultrasonically treated, ultrasonic power is 300~400W, and ultrasonic time is 5~10min.
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| CN110205038A (en) * | 2019-06-19 | 2019-09-06 | 浙江安吉朝辉新材料有限公司 | A kind of environment-friendly type aqueous gluing preparation process |
| CN110218523A (en) * | 2019-06-19 | 2019-09-10 | 浙江安吉朝辉新材料有限公司 | A kind of anti-fouling type aqueous gluing production technology |
| CN110283536A (en) * | 2019-06-19 | 2019-09-27 | 浙江安吉朝辉新材料有限公司 | A kind of process for producing of novel glue |
| CN112980358A (en) * | 2021-03-04 | 2021-06-18 | 吉安迅达科技有限公司 | Environment-friendly energy-saving adhesive and preparation method thereof |
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| CN101798491B (en) * | 2010-02-25 | 2012-05-30 | 北京高盟新材料股份有限公司 | Pressure sensitive adhesive for protective film and preparation method thereof |
| CN101864257B (en) * | 2010-05-26 | 2012-07-25 | 北京高盟新材料股份有限公司 | Adhesive for automobile adhesive film and preparation method thereof |
| KR101748015B1 (en) * | 2014-12-19 | 2017-06-15 | 삼성에스디아이 주식회사 | Adhesive composition for polarizing plate, polarizing plate comprising the same and optical display apparatus comprising the same |
| CN105602492A (en) * | 2015-12-30 | 2016-05-25 | 安徽明讯新材料科技股份有限公司 | Application method of solvent type polymethacrylate pressure-sensitive adhesive |
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