CN104479616A - Adhesive with strong adhesion performance and preparation method thereof - Google Patents
Adhesive with strong adhesion performance and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an adhesive with strong adhesion performance and a preparation method thereof, and belongs to the technical field of adhesive for leather products. The preparation method comprises the following four steps: 1, preparing a compound 1 by means of a di-hydroxyl protection reaction; 2, preparing a compound 2 by means of an activated fat activation reaction; 3, preparing a compound 3 by means of an amidation reaction; and 4, synthesizing the adhesive with strong adhesion performance. According to the preparation method, a novel adhesive of functional compound dopamine is firstly synthesized, and the adhesive is combined with advantages of polyurethane and dopamine, has strong adhesion performance, is suitable for adhesion of leather materials, and has the characteristics of durable firmness and aging prevention.
Description
Technical field
The present invention relates to a kind of tackiness agent and preparation method thereof, specifically a kind of tackiness agent and preparation method thereof of strong bond properties, belongs to leatherware technical field of adhesive.
Background technology
The main chemical structure characteristic of urethane is containing a large amount of carbamate groups repeated in its main chain.Polyurethane backbone is formed higher than the hard section of the room temperature block that is alternately arranged lower than soft section of room temperature and second-order transition temperature by second-order transition temperature.Its general structure is-(A-B) n-.Wherein A representative is hard section, forms for various isocyanic ester and small molecule chain extender (binary or polyvalent alcohol or amine) react; What B represented is soft section.In PU, incompatible due to soft section and hard section, cause there is obvious micro phase separation structure in urethane, wherein hard section plays mutually to strengthen and fills and crosslinked action, and the urethane that act as of soft section of phase provides elasticity.This polymer with heterogeneous structure has the good characteristics such as excellent high rigidity, physical strength, chemical resistance and abrasion performance.Due to the polar character of carbamate groups (-NHCOO-), the ability of hydrogen bond is formed and deliquescent difference between soft section and hard section between polyurethanyl group, cause the flexible polyurethane section phenomenon that therefore produce microphase-separated incompatible with hard section thermodynamics, because the effect strong associations of hydrogen bond is dispersed in soft section of phase matrix together between hard segment molecule.The polyurethane material formed not is so-called random copolymers, but a kind of " mixture ".There is the hard section of strong polarity and hydrogen bond action in the soft segment base matter of rubbery state, play the effect of physical crosslinking point and active-reinforcing fillers in urethane.
Due to the isocyanate group (-NCO) containing a large amount of very extensive chemical activity and strong polarity and carbamate groups (-NHCOO-) in polyurethane adhesives, therefore with the material containing reactive hydrogen, as the porous materials such as porous plastics, leather, pottery, timber, paper, fabric and metal, rubber, the material of any surface finish such as resin glass has excellent cohesive strength.Meanwhile, the hydrogen bond action that urethane can produce between base material can improve intermolecular forces interaction force, strengthens bonding strength therebetween.
The tackiness agent that different hardness and elongation require can be made by regulating soft or hard section ratio and structure in formula, change molecular chain.By regulating preparation different types of tamanori from flexibility to rigidity, thus the gluing of differing materials can be met.
Polyurethane adhesive is synthetic adhesive industry staple product class, is widely used in all fields of national economy.Because it contains active function groups-NCO base in tackiness agent, therefore can improve the agglutinating value(of coal) to various material, and there is very high reactivity, can normal temperature aftertreatment be carried out.Glued membrane is tough and tensile, flexibility is good, stripping strength is high, shock-resistant, there is good resistance to ultralow warm nature, oil resistant and wear resistance etc., therefore it not only can glued joint polyurethane sponge and urethanes, and rubber and metal, metal and metal, rubber and fabric, timber and timber, metal and ceramic and rubber and plastics etc. can be gluedd joint.
Chinese invention: CN201180020170.0; The invention provides the starch mixture prepared for coating composition, and with the coating composition that it is prepared, be characterised in that this starch mixture comprises (a) non-rare solution starch; (b) rare solution starch.But this invention is not also suitable for the bonding of leatherware material.Therefore, develop the tackiness agent tool being applicable to leatherware material to be of great significance.
Summary of the invention
The object of this invention is to provide tackiness agent of a kind of strong bond properties and preparation method thereof, this manufacture method first synthesizes a kind of new type bonding agent of novel functional compounds Dopamine HCL, the advantage of both urethane and Dopamine HCL combines by this tackiness agent, obtain a kind of bond properties strong, be applicable to the bonding of leatherware material, firmly long-term, feature that can not be aging.
Object of the present invention is achieved by the following technical programs:
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
2, 2-hydroxymethyl propionic acid 10-30 part, 2, 2-Propanal dimethyl acetal 10-30 part, acetone 10-20 part, to methylsulphonic acid 20-30 part, sodium bicarbonate 20-30 part, N-hydroxy-succinamide 20-40 part, methylene dichloride 15-30 part, 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate 20-35 part, dilute hydrochloric acid 30-50 part, magnesium sulfate 20-35 part, methyl alcohol 10-40 part, dopamine hydrochloride 20-40 part, triethylamine 10-20 part, diphenylmethanediisocyanate 20-40 part, PTMG 20-30 part, 1, 4-butyleneglycol 20-40 part, N, dinethylformamide 10-30 part,
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction: by 2,2-hydroxymethyl propionic acid, 2,2-Propanal dimethyl acetal adds in single port flask, adds acetone and makes it dissolve, then add methylsulphonic acid, room temperature lower magnetic force stirring reaction 3-6 h, add sodium bicarbonate neutralization, stir 10-40 min, filter and obtain clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2: compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 1-4h, then room temperature reaction 20-30 h; First wash 2-5 time with saturated sodium bicarbonate solution, then wash 2-5 time with dilute hydrochloric acid solution, finally wash 2-5 time with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 10-40min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3: get methylene dichloride and methyl alcohol is added in there-necked flask, add dopamine hydrochloride again, stir for some time, add triethylamine again, stir for some time, then add compound 2, ice bath reaction 20-30h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties: diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 40-80 DEG C; 2-6h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 40-60 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
The present invention relative to the beneficial effect of prior art is:
Compared with additive method, this manufacture method first synthesizes a kind of new type bonding agent of novel functional compounds Dopamine HCL, and the advantage of both urethane and Dopamine HCL combines by this tackiness agent, obtain a kind of bond properties strong, be applicable to the bonding of leatherware material, for a long time firmly, feature that can not be aging.
The thermal weight loss data of this product:
| Project | Product |
| Hard section temperature of initial decomposition/DEG C | 309.76 |
| Soft section of temperature of initial decomposition/DEG C | 407.18 |
| Carbon left/% | 3.89 |
The shear adhesive strength of this product on leatherware:
| This product | Common adhesive | |
| Shear adhesive strength/MPa | 0.21 | 0.16 |
Embodiment
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention, the specific embodiment of the invention is implemented by Synthesis and applications two aspect.
Embodiment 1
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
10 part 2,2-hydroxymethyl propionic acid, 10 part 2,2-Propanal dimethyl acetal, 10 parts of acetone, 20 parts to methylsulphonic acid, 20 parts of sodium bicarbonates, 20 parts of N-hydroxy-succinamides, 15 parts of methylene dichloride, 20 parts of 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorates, 30 parts of dilute hydrochloric acid, 20 parts of magnesium sulfate, 10 parts of methyl alcohol, 20 parts of dopamine hydrochlorides, 10 parts of triethylamines, 20 parts of diphenylmethanediisocyanates, 20 parts of PTMG, 20 part 1,4-butyleneglycol, 10 parts of DMFs;
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction:
2,2-hydroxymethyl propionic acid, 2,2-dimethoxypropane are added in single port flask, adds acetone and make it dissolve, add again methylsulphonic acid, room temperature lower magnetic force stirring reaction 3h, add sodium bicarbonate neutralization, stir 10 min, filtration obtains clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2:
Compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 1h, then room temperature reaction 20 h; First wash 2 times with saturated sodium bicarbonate solution, then wash 2 times with dilute hydrochloric acid solution, finally wash 2 times with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 10min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3:
Get methylene dichloride and methyl alcohol is added in there-necked flask, then add dopamine hydrochloride, stir for some time, then add triethylamine, stir for some time, then add compound 2, ice bath reaction 20h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties:
Diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 40 DEG C; 2h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 40 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
Embodiment 2
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
15 part 2,2-hydroxymethyl propionic acid, 15 part 2,2-Propanal dimethyl acetal, 15 parts of acetone, 25 parts to methylsulphonic acid, 25 parts of sodium bicarbonates, 25 parts of N-hydroxy-succinamides, 20 parts of methylene dichloride, 25 parts of 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorates, 35 parts of dilute hydrochloric acid, 25 parts of magnesium sulfate, 15 parts of methyl alcohol, 25 parts of dopamine hydrochlorides, 15 parts of triethylamines, 25 parts of diphenylmethanediisocyanates, 25 parts of PTMG, 25 part 1,4-butyleneglycol, 15 parts of DMFs;
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction:
2,2-hydroxymethyl propionic acid, 2,2-dimethoxypropane are added in single port flask, adds acetone and make it dissolve, add again methylsulphonic acid, room temperature lower magnetic force stirring reaction 4h, add sodium bicarbonate neutralization, stir 15min, filtration obtains clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2:
Compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 2h, then room temperature reaction 25 h; First wash 3 times with saturated sodium bicarbonate solution, then wash 3 times with dilute hydrochloric acid solution, finally wash 3 times with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 15min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3:
Get methylene dichloride and methyl alcohol is added in there-necked flask, then add dopamine hydrochloride, stir for some time, then add triethylamine, stir for some time, then add compound 2, ice bath reaction 25h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties:
Diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 45 DEG C; 3h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 45 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
Embodiment 3
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
20 part 2,2-hydroxymethyl propionic acid, 20 part 2,2-Propanal dimethyl acetal, 20 parts of acetone, 30 parts to methylsulphonic acid, 30 parts of sodium bicarbonates, 30 parts of N-hydroxy-succinamides, 30 parts of methylene dichloride, 30 parts of 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorates, 40 parts of dilute hydrochloric acid, 30 parts of magnesium sulfate, 20 parts of methyl alcohol, 30 parts of dopamine hydrochlorides, 20 parts of triethylamines, 30 parts of diphenylmethanediisocyanates, 30 parts of PTMG, 30 part 1,4-butyleneglycol, 20 parts of DMFs;
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction:
2,2-hydroxymethyl propionic acid, 2,2-dimethoxypropane are added in single port flask, adds acetone and make it dissolve, add again methylsulphonic acid, room temperature lower magnetic force stirring reaction 5 h, add sodium bicarbonate neutralization, stir 340 min, filtration obtains clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2:
Compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 3h, then room temperature reaction 30 h; First wash 4 times with saturated sodium bicarbonate solution, then wash 4 times with dilute hydrochloric acid solution, finally wash 4 times with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 30min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3:
Get methylene dichloride and methyl alcohol is added in there-necked flask, then add dopamine hydrochloride, stir for some time, then add triethylamine, stir for some time, then add compound 2, ice bath reaction 30h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties:
Diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 60 DEG C; 4h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 50 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
Embodiment 4
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
25 part 2,2-hydroxymethyl propionic acid, 25 part 2,2-Propanal dimethyl acetal, 10 parts of acetone, 20 parts to methylsulphonic acid, 20 parts of sodium bicarbonates, 20 parts of N-hydroxy-succinamides, 30 parts of methylene dichloride, 35 parts of 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorates, 50 parts of dilute hydrochloric acid, 35 parts of magnesium sulfate, 40 parts of methyl alcohol, 40 parts of dopamine hydrochlorides, 20 parts of triethylamines, 40 parts of diphenylmethanediisocyanates, 30 parts of PTMG, 40 part 1,4-butyleneglycol, 30 parts of DMFs;
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction:
2,2-hydroxymethyl propionic acid, 2,2-dimethoxypropane are added in single port flask, adds acetone and make it dissolve, add again methylsulphonic acid, room temperature lower magnetic force stirring reaction 5 h, add sodium bicarbonate neutralization, stir 40 min, filtration obtains clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2:
Compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 4h, then room temperature reaction 30 h; First wash 5 times with saturated sodium bicarbonate solution, then wash 5 times with dilute hydrochloric acid solution, finally wash 5 times with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 40min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3:
Get methylene dichloride and methyl alcohol is added in there-necked flask, then add dopamine hydrochloride, stir for some time, then add triethylamine, stir for some time, then add compound 2, ice bath reaction 30h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties:
Diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 70 DEG C; 6h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 60 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
Embodiment 5
A tackiness agent for strong bond properties, this tackiness agent is made up of the composition of following weight part:
30 part 2,2-hydroxymethyl propionic acid, 10 part 2,2-Propanal dimethyl acetal, 20 parts of acetone, 30 parts to methylsulphonic acid, 30 parts of sodium bicarbonates, 40 parts of N-hydroxy-succinamides, 15 parts of methylene dichloride, 20 parts of 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorates, 30 parts of dilute hydrochloric acid, 20 parts of magnesium sulfate, 40 parts of methyl alcohol, 40 parts of dopamine hydrochlorides, 10 parts of triethylamines, 40 parts of diphenylmethanediisocyanates, 30 parts of PTMG, 40 part 1,4-butyleneglycol, 10 parts of DMFs;
A manufacture method for the tackiness agent of strong bond properties, comprises the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction:
2,2-hydroxymethyl propionic acid, 2,2-dimethoxypropane are added in single port flask, adds acetone and make it dissolve, add again methylsulphonic acid, room temperature lower magnetic force stirring reaction 6 h, add sodium bicarbonate neutralization, stir 40 min, filtration obtains clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2:
Compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 4h, then room temperature reaction 30 h; First wash 2 times with saturated sodium bicarbonate solution, then wash 3 times with dilute hydrochloric acid solution, finally wash 5 times with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 10-40min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3:
Get methylene dichloride and methyl alcohol is added in there-necked flask, then add dopamine hydrochloride, stir for some time, then add triethylamine, stir for some time, then add compound 2, ice bath reaction 30h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties:
Diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 80 DEG C; 6h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 60 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
Claims (2)
1. a tackiness agent for strong bond properties, is characterized in that: this tackiness agent is made up of the composition of following weight part:
2, 2-hydroxymethyl propionic acid 10-30 part, 2, 2-Propanal dimethyl acetal 10-30 part, acetone 10-20 part, to methylsulphonic acid 20-30 part, sodium bicarbonate 20-30 part, N-hydroxy-succinamide 20-40 part, methylene dichloride 15-30 part, 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate 20-35 part, dilute hydrochloric acid 30-50 part, magnesium sulfate 20-35 part, methyl alcohol 10-40 part, dopamine hydrochloride 20-40 part, triethylamine 10-20 part, diphenylmethanediisocyanate 20-40 part, PTMG 20-30 part, 1, 4-butyleneglycol 20-40 part, N, dinethylformamide 10-30 part.
2. a manufacture method for the tackiness agent of strong bond properties, is characterized in that: comprise the following steps:
(1) compound 1 is prepared in two hydroxyl protection reaction: by 2,2-hydroxymethyl propionic acid, 2,2-Propanal dimethyl acetal adds in single port flask, adds acetone and makes it dissolve, then add methylsulphonic acid, room temperature lower magnetic force stirring reaction 3-6 h, add sodium bicarbonate neutralization, stir 10-40 min, filter and obtain clear liquid, concentrating under reduced pressure, obtains white compound 1;
(2) activate fat priming reaction and prepare compound 2: compound 1 and N-hydroxy-succinamide are added in single port flask, adding methylene dichloride makes it dissolve, add 1-ethyl-(3-dimethylaminopropyl) phosphinylidyne diimmonium salt hydrochlorate again, first ice bath reaction 1-4h, then room temperature reaction 20-30 h; First wash 2-5 time with saturated sodium bicarbonate solution, then wash 2-5 time with dilute hydrochloric acid solution, finally wash 2-5 time with deionized water, isolate after organic phase adds anhydrous magnesium sulfate drying 10-40min and filter, obtain white powder compound 2;
(3) amidate action prepares compound 3: get methylene dichloride and methyl alcohol is added in there-necked flask, add dopamine hydrochloride again, stir for some time, add triethylamine again, stir for some time, then add compound 2, ice bath reaction 20-30h, underpressure distillation obtains yellow viscous substance, with dilute hydrochloric acid solution washing, obtains compound 3 after drying;
(4) the tackiness agent synthesis of strong bond properties: diphenylmethanediisocyanate and PTMG are added in there-necked flask and carry out prepolymerization reaction; at 40-80 DEG C; 2-6h is reacted under nitrogen protection; by the content of-NCO in toluene-Di-n-Butyl Amine method mensuration system; compound 3 and 1 is added in prepolymer; the mixed chain extender of 4-butyleneglycol; add N; dinethylformamide, at 40-60 DEG C, carries out chain extending reaction under nitrogen protection; treat that product cools; under agitation solution is slowly poured into precipitation in diluted hydrochloric acid aqueous solution and obtains product, vacuum-drying.
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| CN107325751A (en) * | 2017-08-07 | 2017-11-07 | 安徽凤凰松包装有限公司 | A kind of corrugated paper anti-aging amylum adhesive |
| CN109796576A (en) * | 2019-01-07 | 2019-05-24 | 泰山玻璃纤维有限公司 | A kind of glass fibre film forming agent and preparation method thereof |
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| CN115651592A (en) * | 2022-11-10 | 2023-01-31 | 福建师范大学 | Adhesive capable of being used underwater and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106010416A (en) * | 2016-05-28 | 2016-10-12 | 上海大学 | Polyurethane adhesive system based on D-A reaction and preparation method of polyurethane adhesive system |
| CN106010416B (en) * | 2016-05-28 | 2019-01-11 | 上海大学 | The polyurethane gluing system and preparation method thereof constructed based on diels-Alder reaction |
| CN107325751A (en) * | 2017-08-07 | 2017-11-07 | 安徽凤凰松包装有限公司 | A kind of corrugated paper anti-aging amylum adhesive |
| CN109796576A (en) * | 2019-01-07 | 2019-05-24 | 泰山玻璃纤维有限公司 | A kind of glass fibre film forming agent and preparation method thereof |
| CN111253543A (en) * | 2020-01-21 | 2020-06-09 | 西安医学院 | Novel MAP medical adhesive material based on biomimetic synthesis and preparation method thereof |
| CN112210337A (en) * | 2020-09-30 | 2021-01-12 | 丁建利 | Adhesive for bonding metal and plastic and preparation method thereof |
| CN115651592A (en) * | 2022-11-10 | 2023-01-31 | 福建师范大学 | Adhesive capable of being used underwater and preparation method thereof |
| CN115651592B (en) * | 2022-11-10 | 2024-01-26 | 福建师范大学 | Adhesive capable of being used underwater and preparation method thereof |
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