CN113527636A - Preparation method of low-viscosity environment-friendly high-toughness epoxy curing agent - Google Patents
Preparation method of low-viscosity environment-friendly high-toughness epoxy curing agent Download PDFInfo
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- CN113527636A CN113527636A CN202110817679.3A CN202110817679A CN113527636A CN 113527636 A CN113527636 A CN 113527636A CN 202110817679 A CN202110817679 A CN 202110817679A CN 113527636 A CN113527636 A CN 113527636A
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- curing agent
- epoxy resin
- diglycidyl ether
- butanediol diglycidyl
- diethylenetriamine
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 81
- 239000004593 Epoxy Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 84
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 84
- SHKUUQIDMUMQQK-UHFFFAOYSA-N 2-[4-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COCCCCOCC1CO1 SHKUUQIDMUMQQK-UHFFFAOYSA-N 0.000 claims abstract description 73
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000376 reactant Substances 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 36
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims abstract description 24
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 81
- 238000006243 chemical reaction Methods 0.000 claims description 62
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 11
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 6
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 239000004634 thermosetting polymer Substances 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 2
- 125000003277 amino group Chemical group 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 229920006332 epoxy adhesive Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- RYYVLZVUVIJVGH-UHFFFAOYSA-N trimethylxanthine Natural products CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 1
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- 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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
-
- 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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/182—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing using pre-adducts of epoxy compounds with curing agents
- C08G59/184—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing using pre-adducts of epoxy compounds with curing agents with amines
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to the technical field of epoxy resin curing agents, in particular to a preparation method of a low-viscosity environment-friendly high-toughness epoxy curing agent, which comprises the following steps: the raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are mixed to be used as addition reactants, the diepoxy-terminated and ether bond in the molecular structural formula of the 1, 4-butanediol diglycidyl ether can improve the toughness of the curing agent, and because the epoxy equivalent of the 1, 4-butanediol diglycidyl ether is small, the active hydrogen atom number on the amino group of diethylenetriamine consumed as the reactants is twice of that of the E51 epoxy resin with the same molar mass, the micromolecular amine and free amine in the curing agent can be reduced, thereby reducing the odor and the toxicity.
Description
Technical Field
The invention relates to the technical field of curing agents, in particular to a preparation method of a low-viscosity environment-friendly high-toughness epoxy curing agent
Background
Epoxy resin paint is widely applied to the coating field due to the properties of high hardness, good wear resistance, high adhesive force, chemical resistance and the like. The epoxy adhesive mainly comprises epoxy resin, a curing agent, a filler and the like, wherein the curing agent is a key factor influencing the bonding strength and toughness of the epoxy adhesive. However, the existing preparation method for performing addition modification on the E51 epoxy resin has the defects of high content of free amine and small molecular amine of a curing agent, high toxicity, heavy smell, poor toughness, high viscosity, inconvenience for normal temperature use, potential safety hazard in the production and use processes and influence on the product practicability, and the problem is solved by providing the preparation method for the low-viscosity environment-friendly high-toughness epoxy curing agent.
SUMMARY OF THE PATENT FOR INVENTION
The invention aims to provide a preparation method of a low-viscosity environment-friendly high-toughness epoxy curing agent, which solves the problems that the existing preparation method adopting E51 epoxy resin for addition modification has high content of free amine and micromolecule amine of the curing agent, higher toxicity, heavier smell, poorer toughness, high viscosity, inconvenience for normal temperature use, potential safety hazard in the production and use process and influence on the practicability of products.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a low-viscosity environment-friendly high-toughness epoxy curing agent comprises the following steps:
step 1: the raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin;
step 2: preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant;
and step 3: preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Preferably, theIn step 1, benzyl alcohol is an organic compound of formula C7H8O is aromatic alcohol.
Preferably, in step 1, the molecular formula of diethylenetriamine is C4H13N3Yellow, transparent, viscous liquid with hygroscopicity.
Preferably, in step 1, the 1, 4-butanediol diglycidyl ether is an epoxy resin containing a 1, 4-butanediol diglycidyl ether chain and is prepared by polycondensation of 1, 4-butanediol and epichlorohydrin, and the 1, 4-butanediol diglycidyl ether is an addition-modified product.
Preferably, in step 1, the E51 epoxy resin is one of epoxy resins, and is a thermosetting polymer composite material.
Preferably, after the curing agent is prepared in the step 3, the vacuum degree in the temperature-controlled reaction kettle is increased by performing reduced pressure dehydration, when the fraction is less, the temperature in the temperature-controlled reaction kettle is gradually increased, and after the curing agent reaches a stable amine value, the distillation is stopped.
Preferably, in step 3, the finished product is cooled and finally barreled.
Preferably, in step 3, when the epoxy resin and the curing agent need to be prepared for application, the application ratio of the epoxy resin to the curing agent is 100: 50.
compared with the prior art, the invention has the following beneficial effects:
the invention takes 1, 4-butanediol diglycidyl ether and E51 epoxy resin as addition reactants after being mixed, the dual epoxy group end capping and ether bond in the molecular structural formula of the 1, 4-butanediol diglycidyl ether can improve the toughness of the curing agent, and because the epoxy equivalent of the 1, 4-butanediol diglycidyl ether is small, the active hydrogen atom number on the diethylenetriamine amino group consumed as the reactants is twice of that of the E51 epoxy resin with the same molar mass, the micromolecule amine and free amine in the curing agent can be reduced, thereby reducing the odor and the toxicity.
Drawings
FIG. 1 is a flow chart of the inventive patent architecture;
FIG. 2 shows the chemical reaction mechanism of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by a person skilled in the art based on the embodiments in the patent of the invention without any inventive work belong to the protection scope of the patent of the invention.
Referring to fig. 1-2, a method for preparing a low-viscosity environment-friendly high-toughness epoxy curing agent includes the following steps:
step 1: the raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin;
step 2: preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant;
and step 3: preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
The first embodiment is as follows:
the raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example two:
in the first embodiment, the following steps are added:
in step 1, benzyl alcohol is an organic compound of formula C7H8O, an aromatic alcohol, reduces the viscosity of the curing agent and increases the rate of addition reaction.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example three:
in the second embodiment, the following steps are added:
in step 1, the molecular formula of diethylenetriamine is C4H13N3The yellow transparent viscous liquid with hygroscopicity can be well crosslinked and cured with E51 epoxy resin at normal temperature.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example four:
in the third embodiment, the following steps are added:
in the step 1, 4-butanediol diglycidyl ether is epoxy resin containing 1, 4-butanediol diglycidyl ether chains and prepared by polycondensation of 1, 4-butanediol and epichlorohydrin, and the 1, 4-butanediol diglycidyl ether is an added-layer modifier, so that the use amount of E51 epoxy resin can be reduced, the toxicity of a curing agent is reduced, and the mechanical property can be improved
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example five:
in the fourth example, the following steps were added:
in step 1, the E51 epoxy resin is one of epoxy resins, is a thermosetting polymer composite material, and has high strength and hardness after being cured.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example six:
in the fifth example, the following steps were added:
in step 3, after the curing agent is prepared, pressure reduction and dehydration are carried out, the vacuum degree in the temperature control reaction kettle is improved, when the fraction is less, the temperature in the temperature control reaction kettle is gradually improved, and after the curing agent reaches a stable amine value, distillation is stopped, so that the subsequent product quality is ensured.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example seven:
in example six, the following steps were added:
in step 3, the finished product is cooled and finally barreled, so that the subsequent use is facilitated.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
Example eight:
in example seven, the following steps were added:
in step 3, when the epoxy resin and the curing agent need to be prepared for application, the application ratio of the epoxy resin to the curing agent is 100: 50, the effect of the product can be effectively exerted.
The raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin; preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant; preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
It should be noted that:
the structural formula of diethylenetriamine is as follows:
H2N-(CH2)2-NH-(CH2)2-NH2
the structural formula of benzyl alcohol is:
the structural formula of the E51 epoxy resin is as follows:
the structural formula of the 1, 4-butanediol diglycidyl ether is as follows:
although embodiments of the present patent have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the present patent, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of a low-viscosity environment-friendly high-toughness epoxy curing agent is characterized by comprising the following steps: the method comprises the following steps:
step 1: the raw material components are as follows: raw materials of the curing agent comprise benzyl alcohol, diethylenetriamine, 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the raw materials respectively account for 23-29g of benzyl alcohol, 10-14g of diethylenetriamine, 2.5-4.5g of 1, 4-butanediol diglycidyl ether and 8-10g of E51 epoxy resin;
step 2: preparing a primary reactant: firstly adding benzyl alcohol into a temperature control reaction kettle, then adding diethylenetriamine into the temperature control reaction kettle, wherein the adding amount of the benzyl alcohol is 23-29g, the adding amount of the diethylenetriamine is 10-14g, starting the temperature control reaction kettle, controlling the temperature at 60 ℃, and reacting to prepare a primary reactant;
and step 3: preparing a curing agent: respectively introducing 1, 4-butanediol diglycidyl ether and E51 epoxy resin into a dripping pipeline, aligning the discharge end of the dripping pipeline to a primary reactant in a temperature-controlled reaction kettle, dripping 1, 4-butanediol diglycidyl ether and E51 epoxy resin, wherein the addition amounts of the 1, 4-butanediol diglycidyl ether and the E51 epoxy resin are respectively 2.5-4.5g and 8-10g, and carrying out mixed reaction for 4 hours to prepare the curing agent.
2. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: in step 1, the benzyl alcohol is an organic compound of formula C7H8O is aromatic alcohol.
3. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: in the step 1, the molecular formula of the viscous triamine is C4H13N3Yellow, transparent viscous liquid with hygroscopicity.
4. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: in the step 1, 4-butanediol diglycidyl ether is epoxy resin containing 1, 4-butanediol diglycidyl ether chains and is prepared by polycondensation of 1, 4-butanediol and epichlorohydrin, and the 1, 4-butanediol diglycidyl ether is an addition layer modifier.
5. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: in step 1, the E51 epoxy resin is one of epoxy resins, and is a thermosetting polymer composite material.
6. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: and 3, after the curing agent is prepared, decompressing and dewatering to improve the vacuum degree in the temperature-control reaction kettle, gradually increasing the temperature in the temperature-control reaction kettle when the fraction is less, and stopping distillation after the curing agent reaches a stable amine value.
7. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: and in the step 3, cooling after the finished product is prepared, and finally barreling.
8. The method for preparing the low-viscosity environment-friendly high-toughness epoxy curing agent as claimed in claim 1, wherein the curing agent comprises the following components in percentage by weight: in the step 3, when the epoxy resin and the curing agent are required to be prepared and applied, the application ratio of the epoxy resin to the curing agent is 100: 50.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608826A (en) * | 2015-11-22 | 2017-05-03 | 宁夏际华环境安全科技有限公司 | Production technology of epoxy curing agent |
| CN106893451A (en) * | 2017-03-09 | 2017-06-27 | 烟台大学 | A kind of epoxy paste paint and its preparation application method without nonyl phenol |
| CN109280521A (en) * | 2018-09-30 | 2019-01-29 | 武汉市石代高新建材有限公司 | A kind of epoxy structural rubber curing agent and its preparation method and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608826A (en) * | 2015-11-22 | 2017-05-03 | 宁夏际华环境安全科技有限公司 | Production technology of epoxy curing agent |
| CN106893451A (en) * | 2017-03-09 | 2017-06-27 | 烟台大学 | A kind of epoxy paste paint and its preparation application method without nonyl phenol |
| CN109280521A (en) * | 2018-09-30 | 2019-01-29 | 武汉市石代高新建材有限公司 | A kind of epoxy structural rubber curing agent and its preparation method and application |
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Application publication date: 20211022 |