CN107254281A - A kind of preparation method for the water-fast epoxy resin being bonded for dalle - Google Patents
A kind of preparation method for the water-fast epoxy resin being bonded for dalle Download PDFInfo
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- CN107254281A CN107254281A CN201610995156.7A CN201610995156A CN107254281A CN 107254281 A CN107254281 A CN 107254281A CN 201610995156 A CN201610995156 A CN 201610995156A CN 107254281 A CN107254281 A CN 107254281A
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- epoxy resin
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Classifications
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
-
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Epoxy Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation method for the water-fast epoxy resin being bonded for dalle, concretely comprise the following steps：1）Preparation prepares the raw material of bisphenol-s epoxy resin first, then prepares bisphenol-s epoxy resin stand-by；2）Then the modification operation of bisphenol-s epoxy resin is carried out, addition modifying agent and the bisphenol-s epoxy resin prepared carry out heating response, and obtain modified epoxy；3）Then mixed curing agent is prepared, the mixed curing agent includes 52 83 parts of dodecenylsuccinic anhydride curing agent, 18 32 parts of dimethylformamide, 28 42 parts of filler, 19 27 parts of liquid polysulfide rubber, 17 32 parts of dimethyl methyl phosphonate；4）After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.The present invention controls reaction condition by rationally controlling the proportioning between each reactant, rationally and prepares a kind of High-durability epoxy resin adhesive for applying to light industry and textile industry.
Description
Technical field
The present invention relates to high-molecular gel field, a kind of water-fast epoxy resin being bonded for dalle is specifically referred to
Preparation method.
Background technology
The adhesive product that house decoration adhesive is commonly used as light industry industry is widely used in decoration plastics or wooden
Material processing and other fields, for house decoration, need to use bonding agent when being bonded multilayer material.And it is conventional at present general
Logical bonding agent usually contains the organic poisons such as aldehydes, and its release can influence health.So, how to solve general adhesive and release
Put the technical problem that dusty gas is urgent need to resolve.
And epoxyn as a kind of environment-friendly type gel rubber material the problem of can solve the problem that existing building adhesive, institute
The epoxyn stated is the work that a class is formulated by epoxy resin base-material, curing agent, diluent, accelerator and filler
Journey adhesive.Because its adhesive property is good, feature is good, less expensive, technique for sticking easy, so existing in recent decades
Household electrical appliances, automobile, water conservancy traffic, electronic apparatus and aerospace industry field are widely used.With new and high technology and nanometer
Technology is continued to develop, and in recent years, the modification to epoxy resin deepens continuously, and interpenetrating networks, chemical copolymerization and nano-particle increase
The method extensive use such as tough, by epoxy preparation into various high-performance adhesive kinds it is also more and more.But it has one
Individual obvious shortcoming is toughness deficiency, easily poor impact resistance, cracking after solidification, and the shortcoming greatly limit answering for epoxy resin
With.The characteristic requirements more and more highers developed rapidly to epoxy resin of various materials, epoxy resin is solidified into epoxy resin
The emphasis of use research, people carry out solidification toughness reinforcing using a variety of methods to epoxy resin, so that its application field is more
Extensively.
The content of the invention
Dalle bonding is used in it is an object of the invention to provide a kind of and with the adhesive of efficient water-fast function
Preparation method.
The present invention is achieved through the following technical solutions：A kind of preparation side for the water-fast epoxy resin being bonded for dalle
Method, is concretely comprised the following steps：
（1）Preparation prepares the raw material of bisphenol-s epoxy resin first, then prepares bisphenol-s epoxy resin stand-by；
（2）Then the modification operation of bisphenol-s epoxy resin, addition modifying agent and the bisphenol-s epoxy resin prepared are carried out
Heating response is carried out, and obtains modified epoxy；
（3）Then mixed curing agent is prepared, the mixed curing agent includes 52-83 parts of dodecenylsuccinic anhydride curing agent, two
18-32 parts of NMF, 28-42 parts of filler, 19-27 parts of liquid polysulfide rubber, 17-32 parts of dimethyl methyl phosphonate；
（4）After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
Further, the step（1）It is middle to prepare concretely comprising the following steps for bisphenol-s epoxy resin：
（1.1）Prepare raw material, the raw material is sodium hydroxide, epoxychloropropane, hydrogenated bisphenol A and methyl iso-butyl ketone (MIBK)；
（1.2）Represented with parts by weight, take 11-18 parts of sodium hydroxide, 24-39 parts of epoxychloropropane, 16-24 parts of bisphenol S,
19-27 parts of methyl iso-butyl ketone (MIBK) is simultaneously added in reactor, and add catalyst by a certain percentage, then 42-55 DEG C of thermostatted water
Bathe and stir；Then condensing reflux reacts 21h；
（1.3）Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, after then upper aqueous layer is filtered out
Surplus solution is heated to 78 DEG C and sodium hydroxide solution is added, then constant temperature stirring reaction 1-2.5h；
（1.4）Distilled water washing point liquid is added after question response, until when the water layer pH value separated is neutral, filtrate is completely distilled off
Later, light yellow, transparent bisphenol-s epoxy resin is obtained.
It is preferred that, the step（1.3）In sodium hydroxide mass fraction be 34-37%, the step（1.4）In
Vapo(u)rizing temperature is 95-96 DEG C.
Further, the step（2）In modification operation concretely comprise the following steps：
（2.1）Modifying agent is got out, the modifying agent is vinyl acetate latex and dibutyl phthalate latex, by two kinds
Dry for standby after latex demulsification；
（2.2）Then vinyl acetate latex is added in bisphenol-s epoxy resin, then for 120-140 DEG C of temperature conditionss
Lower reaction 2-3h；
（2.3）Question response adds dibutyl phthalate latex after terminating, 1- is reacted under 120-140 DEG C of temperature conditionss
1.2h, that is, obtain the modified epoxy for thick liquid under normal temperature.
Further, the step（3）In prepare concretely comprising the following steps for mixed curing agent：
（3.1）Get out mix the raw material of fixative；
（3.2）First take 52-83 parts of dodecenylsuccinic anhydride curing agent, and add 19-27 parts liquid polysulfide rubber and
28-42 parts of filler carries out Hybrid Heating stirring 1-2h, the slow dimethyl methyl for adding 18-32 parts thereto in whipping process
Acid amides；
（3.3）Then the dimethyl methyl phosphonate for adding 17-32 parts continues constant temperature stirring 30-50min, produces mixing and fixes
Agent.
Heretofore described bisphenol-s epoxy resin chemical name be bisphenol-S diglycidyl ether, referred to as BPS or
KGEBS, is in sodium hydroxide catalyzed lower obtained, bisphenol-s epoxy resin heat resistance height, heat by bisphenol S and epoxychloropropane
Deformation temperature 60 ~ 700C solidfied materials higher than bisphenol A epoxide resin cun are stable, and solvent resistance is good.And described laurylene base amber
Amber anhydride curing agent liquid is easily mixed with resin, and working life is long, glue-line good toughness, resistance to sudden heating, good electrical property but drug-resistant
Property it is poor, be at room temperature liquid, easily combined with epoxy resin, be a kind of curing agent commonly used in adhesive.Further, it is described to fill out
Expect for graphite microparticles.
The present invention compared with prior art, with advantages below and beneficial effect：
The method of the present invention by rationally controlling each reactant between proportioning, rationally control reaction condition and prepare a kind of height
Solidify obtained from endurance quality epoxy resin adhesive, the epoxy resin composition that epoxy resin of the invention is obtained
Thing, with the mechanical properties such as moisture-proof, excellent heat resistance, and impact resistance also excellent performance, adhesive property is good, durability
Can be good, and preparation method is simple and easy to apply, is adapted to industrialized production, is compared compared with other epoxy resin adhesives, is bonded without strict
The metal of surface treatment and it is nonmetallic all have good adhesive property and endurance quality, can be applied to adhesive field.
Embodiment
Embodiments of the invention are described below in detail.
Embodiment 1：
A kind of water-fast epoxy resin being bonded for dalle of the present embodiment, is represented with parts by weight, including bisphenol S type epoxy
320-500 parts of resin binder, 52-83 parts of dodecenylsuccinic anhydride curing agent, 18-32 parts of dimethylformamide, filler 28-42
Part, 19-27 parts of liquid polysulfide rubber, 17-32 parts of dimethyl methyl phosphonate.
The preparation method of the present invention, is concretely comprised the following steps：
（1）Preparation prepares the raw material of bisphenol-s epoxy resin first, takes 11-18 parts of sodium hydroxide, 24-39 parts of epoxy
Chloropropane, 16-24 parts of bisphenol S, 19-27 parts of methyl iso-butyl ketone (MIBK) is simultaneously added in reactor by a certain percentage, and addition is urged
Agent, then 42-55 DEG C of water bath with thermostatic control and is stirred；Then condensing reflux reacts 21h；
（2）Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, will after then upper aqueous layer is filtered out
Surplus solution is heated to 78 DEG C and adds sodium hydroxide solution, then constant temperature stirring reaction 1-2.5h；Distillation is added after question response
Water washes a point liquid, until when the water layer pH value separated is neutrality, after filtrate is completely distilled off, obtaining light yellow, transparent pair
Phenol S type epoxy resin；
（4）Then the modification operation of bisphenol-s epoxy resin is carried out, modifying agent is got out, the modifying agent is vinylacetate
Latex and dibutyl phthalate latex, by dry for standby after two kinds of latex demulsifications；Then vinyl acetate latex is added
In bisphenol-s epoxy resin, then 1.8-3.5h is reacted under for 120-140 DEG C of temperature conditionss；Question response is added after terminating
Dibutyl phthalate latex, reacts 1-1.2h under 120-140 DEG C of temperature conditionss, that is, obtains under normal temperature as thick liquid
Modified epoxy；
（5）Then mixed curing agent is prepared by raw material of dodecenylsuccinic anhydride curing agent, 52-83 parts of laurylene is first taken
Base succinic anhydride curing agent, and add 19-27 parts of liquid polysulfide rubber and 28-42 parts of filler progress Hybrid Heating stirring 1-
2h, the slow dimethylformamide for adding 18-32 parts thereto in whipping process；Then 17-32 parts of methylphosphine is added
Dimethyl phthalate continues constant temperature stirring 30-50min, produces mixing fixative；
（6）After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
Embodiment 2：
A kind of water-fast epoxy resin being bonded for dalle of the present embodiment, is represented, the bisphenol S type epoxy with parts by weight
240 parts of resin binder, 39 parts of dodecenylsuccinic anhydride curing agent, 8 parts of dimethylformamide, 18 parts of filler, liquid polysulfide rubber
6 parts of glue, 10 parts of dimethyl methyl phosphonate.
Embodiment 3：
A kind of water-fast epoxy resin being bonded for dalle of the present embodiment, is represented, the bisphenol S type epoxy with parts by weight
310 parts of resin binder, 46 parts of dodecenylsuccinic anhydride curing agent, 12 parts of dimethylformamide, 24 parts of filler, liquid polysulfide rubber
12 parts of glue, 14 parts of dimethyl methyl phosphonate.
Embodiment 4：
A kind of water-fast epoxy resin being bonded for dalle of the present embodiment, is represented, the bisphenol S type epoxy with parts by weight
375 parts of resin binder, 49 parts of dodecenylsuccinic anhydride curing agent, 14 parts of dimethylformamide, 27 parts of filler, liquid polysulfide rubber
17 parts of glue, 15 parts of dimethyl methyl phosphonate.
Then the water-resistant adhesive of three kinds of different formulations ratios of embodiment 2 ~ 4 is subjected to detection contrast, to verify this hair
Bright implementation result.
1st, adhesive strength is tested：Take one group（4）The ligneous piece of same specification, in each ligneous piece, corresponding contact surface is pressed
Every square metre of glue coating of 100g, the specification of each contact surface is 80mm × 40mm, afterwards by the contact surface pair of Liang Ge ligneous pieces
Compression should be overlapped, closed assembly time is no more than 20 minutes, and contact surface applies 0.85-1.20Mpa pressure, and at room temperature, installation time 8 is small
When, place 16 hours after pressure relief, make a strength test again；4 repetitions, average；
2nd, bending strength is tested：Take one group（4）The plastic part of same specification, the modeling referring next to state marked as GB1042-79
Material bend test method is tested, and the specification of every group of plastic part is 100 × 20 × 15mm；
3rd, compressive strength is tested：Take one group（4）The plastic part of same specification, the modeling referring next to state marked as GB1041-79
Material compression test method is tested, and the cross-sectional dimensions for the plastic part tested are 20 × 15mm, a height of 10mm；
4th, water resistance test：Take one group（4）The ligneous piece of same specification, it is every by 100g in the corresponding contact surface of each ligneous piece
Square metre cementing, the specification of each contact surface is 80mm × 40mm, and the contact surface correspondence of Liang Ge ligneous pieces is overlapped into pressure afterwards
Tightly, spontaneously dry 8 hours, soaked in 32-40 DEG C of water, measure is come unglued the time, and 4 repetitions are averaged；
5th, hardening time tests：Take bisphenol-s epoxy resin 5g to be placed in beaker, keep room temperature under conditions of 20-25 DEG C,
Take mixed curing agent 2.0-2.5g to add in beaker, and stir standing after 15-20min and test its hardening time, 4 repetitions are made even
Average.
Table 1
Will according to the adhesive strength of the results showed that embodiment of the present invention 2 ~ 4, bending strength, compressive strength and water resistance
It is better than the comparative example using ordinary epoxy resin adhesive, and hardening time will also be less than ordinary epoxy resin adhesive,
And between three embodiments of the present invention, it can be seen that all test indexs all show the formula rate of the present invention in certain limit
It is interior to reach preferable effect, obvious difference occurs if too small or too big, and pass through to institute by the present invention
There is the collaboration between the adjustment of component proportion, each component, both keep high intensity, there can be preferable water resistance again, with aobvious
The novelty of work.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
A variety of change, modification, replacement and modification can be carried out to these embodiments by departing under the principle and objective of the present invention, of the invention
Scope is limited by claim and its equivalent.
Claims (5)
1. a kind of preparation method for the water-fast epoxy resin being bonded for dalle, it is characterized in that being：Concretely comprise the following steps：
（1）Preparation prepares the raw material of bisphenol-s epoxy resin first, then prepares bisphenol-s epoxy resin stand-by；
（2）Then the modification operation of bisphenol-s epoxy resin, addition modifying agent and the bisphenol-s epoxy resin prepared are carried out
Heating response is carried out, and obtains modified epoxy；
（3）Then mixed curing agent is prepared, the mixed curing agent includes 52-83 parts of dodecenylsuccinic anhydride curing agent, two
18-32 parts of NMF, 28-42 parts of filler, 19-27 parts of liquid polysulfide rubber, 17-32 parts of dimethyl methyl phosphonate；
（4）After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
2. a kind of preparation method of water-fast epoxy resin being bonded for dalle according to claim 1, its feature
It is：The step（1）It is middle to prepare concretely comprising the following steps for bisphenol-s epoxy resin：
（1.1）Prepare raw material, the raw material is sodium hydroxide, epoxychloropropane, hydrogenated bisphenol A and methyl iso-butyl ketone (MIBK)；
（1.2）Represented with parts by weight, take 11-18 parts of sodium hydroxide, 24-39 parts of epoxychloropropane, 16-24 parts of bisphenol S,
19-27 parts of methyl iso-butyl ketone (MIBK) is simultaneously added in reactor, and add catalyst by a certain percentage, then 42-55 DEG C of thermostatted water
Bathe and stir；Then condensing reflux reacts 21h；
（1.3）Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, after then upper aqueous layer is filtered out
Surplus solution is heated to 78 DEG C and sodium hydroxide solution is added, then constant temperature stirring reaction 1-2.5h；
（1.4）Distilled water washing point liquid is added after question response, until when the water layer pH value separated is neutral, filtrate is completely distilled off
Later, light yellow, transparent bisphenol-s epoxy resin is obtained.
3. a kind of preparation method of water-fast epoxy resin being bonded for dalle according to claim 2, its feature
It is：The step（1.3）In sodium hydroxide mass fraction be 34-37%, the step（1.4）In vapo(u)rizing temperature be
95-96℃。
4. a kind of preparation method of water-fast epoxy resin being bonded for dalle according to claim 1, its feature
It is：The step（2）In modification operation concretely comprise the following steps：
（2.1）Modifying agent is got out, the modifying agent is vinyl acetate latex and dibutyl phthalate latex, by two kinds
Dry for standby after latex demulsification；
（2.2）Then vinyl acetate latex is added in bisphenol-s epoxy resin, then for 120-140 DEG C of temperature conditionss
Lower reaction 2-3h；
（2.3）Question response adds dibutyl phthalate latex after terminating, 1- is reacted under 120-140 DEG C of temperature conditionss
1.2h, that is, obtain the modified epoxy for thick liquid under normal temperature.
5. a kind of preparation method of water-fast epoxy resin being bonded for dalle according to claim 1, its feature
It is：The step（3）In prepare concretely comprising the following steps for mixed curing agent：
（3.1）Get out mix the raw material of fixative；
（3.2）First take 52-83 parts of dodecenylsuccinic anhydride curing agent, and add 19-27 parts liquid polysulfide rubber and
28-42 parts of filler carries out Hybrid Heating stirring 1-2h, the slow dimethyl methyl for adding 18-32 parts thereto in whipping process
Acid amides；
（3.3）Then the dimethyl methyl phosphonate for adding 17-32 parts continues constant temperature stirring 30-50min, produces mixing and fixes
Agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610995156.7A CN107254281A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method for the water-fast epoxy resin being bonded for dalle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610995156.7A CN107254281A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method for the water-fast epoxy resin being bonded for dalle |
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| Publication Number | Publication Date |
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| CN107254281A true CN107254281A (en) | 2017-10-17 |
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ID=60028118
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| CN201610995156.7A Withdrawn CN107254281A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method for the water-fast epoxy resin being bonded for dalle |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726045A (en) * | 2013-12-24 | 2015-06-24 | 上海海鹰粘接科技有限公司 | High-temperature resistant flame-retardant epoxy glue and preparation method thereof |
| CN104804693A (en) * | 2015-05-20 | 2015-07-29 | 叶芳 | Novel high temperature-resistant epoxy resin structure adhesive and preparation method thereof |
-
2016
- 2016-11-11 CN CN201610995156.7A patent/CN107254281A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726045A (en) * | 2013-12-24 | 2015-06-24 | 上海海鹰粘接科技有限公司 | High-temperature resistant flame-retardant epoxy glue and preparation method thereof |
| CN104804693A (en) * | 2015-05-20 | 2015-07-29 | 叶芳 | Novel high temperature-resistant epoxy resin structure adhesive and preparation method thereof |
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Application publication date: 20171017 |