CN104592930A - Hot melt adhesive with compression sensitivity and preparation method thereof - Google Patents
Hot melt adhesive with compression sensitivity and preparation method thereof Download PDFInfo
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- CN104592930A CN104592930A CN201510011375.2A CN201510011375A CN104592930A CN 104592930 A CN104592930 A CN 104592930A CN 201510011375 A CN201510011375 A CN 201510011375A CN 104592930 A CN104592930 A CN 104592930A
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Abstract
The invention relates to a hot melt adhesive with compression sensitivity. The high-temperature melt viscosity at the temperature of 150 DEG C is 1500-15000mPa.s, the Shore hardness is 10-40, the tensile strength is 0.1-1MPa, and the elongation at break is more than 1000 percent. The hot melt adhesive is characterized by comprising the following components in percentage by mole through condensation polymerization: 30-45 percent of dimer acids, 5-20 percent of aliphatic dicarboxylic acids, 20-30 percent of aliphatic diamine, 15-25 percent of polyether amine, 0.01-0.06 percent of an end-capping reagent and 0.01-0.1 percent of an acid catalyst, wherein the mole number of the aliphatic dicarboxylic acids is less than or equal to 40 percent of the mole number of the dimer acids. The hot melt adhesive disclosed by the invention has the beneficial effects that the hot melt adhesive with compression sensitivity has high high-temperature melt viscosity, high toughness and high base material adhesion force and is applied to pressure sensitive adhesive tapes and glue in the manufacturing industry.
Description
Technical field
The present invention relates to a kind of hot melt adhesive and preparation method thereof, particularly a kind of polyamide hot with pressure-sensitive and preparation method thereof, belong to adhesive area.
Background technology
Polyamide hot is generally formed by dimeracid, aliphatic dibasic acid and diamine or polyamine polycondensation, has that melting range is narrow, softening temperature is high, nontoxic, oil resistant chemical resistant properties is good, wear resisting property is excellent, the low temperature flexibility high and good to polar material bonding strength.Dimer acid PA hot melt adhesive has very high added value, and market demand is increasing in recent years, has a wide range of applications in industries such as printing packaging, clothes, shoemaking, automotive industry, electronics encapsulation, material contracting with heat and machineries.The representative patents of dimeric acid type polyamide hot melt adhesive has CN102703021, CN102807837, CN103468198 etc., and the polyamide hot that these patents are mentioned highlights the excellent properties of the aspects such as each leisure is high temperature resistant, weathering resistance, bonding force are strong.
Pressure sensitive adhesive (pressure sensitive adhesive, PSA), pressure can be bonding with adherend a little to presser sensor, finger pressure to refer to a class, do not need the class tackiness agent using solvent or other supplementary meanss.Hot-fusible pressure-sensitive adhesive is the third generation pressure sensitive adhesive product after solvent-borne type and emulsion-type pressure-sensitive, and than the above two, thermotropic pressure sensitive glue is solvent-free, more be conducive to environmental protection and safety in production, production efficiency is high, and production cost is relatively low, so current countries in the world positive Devoting Major Efforts To Developing thermotropic pressure sensitive glue.Hot-fusible pressure-sensitive adhesive generally adopts the rubber such as SBS, SIS, polyisobutene or polyacrylate resin to be matrix resin, and open report does not also do the pressure sensitive adhesive of matrix resin about polymeric amide at present.
Summary of the invention
Main purpose of the present invention, aims to provide a kind of polyamide hot with pressure-sensitive and preparation method thereof, and prepared polyamide hot snappiness is high, and substrate bonding power is high, to being applied to the production of thermotropic pressure sensitive sealing tape, sticker.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of hot melt adhesive with pressure-sensitive, high temperature melt viscosity (150 DEG C) is 1500 ~ 15000mPas, shore hardness is 10 ~ 40, tensile strength is 0.1 ~ 1MPa, elongation at break is > 1000%, it is characterized in that: formed by the following composition polycondensation by mole percent: 30% ~ 45% dimeracid, 5% ~ 20% aliphatic dicarboxylic acid, 20% ~ 30% aliphatie diamine, 15% ~ 25% polyetheramine, 0.01% ~ 0.06% end-capping reagent and 0.01% ~ 0.1% acid catalyst, the mole number of described aliphatic dicarboxylic acid is less than or equal to 40% of dimeracid mole number.
Further, this hot melt adhesive high temperature melt viscosity (150 DEG C) is 2000 ~ 13000 mPas; Shore hardness is 15 ~ 35; Tensile strength is 0.15 ~ 0.9MPa; Elongation at break is > 1500%; The molecular fraction of end-capping reagent is 0.01% ~ 0.02%, and the molecular fraction of acid catalyst is 0.05% ~ 0.1%; The mole number of described aliphatic dibasic acid is less than or equal to 35% of dimeracid mole number.
Further, in described dimeracid, mass fraction shared by tripolymer is 5% ~ 10%, mass fraction shared by dimer acids is 80% ~ 90%, mass fraction shared by monomer acids is 5% ~ 10%.
Further, described dimeracid is C16 ~ C20 unsaturated aliphatic dimeracid; Described aliphatic dicarboxylic acid is C6 ~ C12 aliphatic dicarboxylic acid; Described aliphatie diamine is the derivative of C2 ~ C8 aliphatie diamine or C2 ~ C8 aliphatie diamine; Described polyetheramine is for containing 2 ~ 3 Amino End Group, and molecular weight is the polyether polyamine of 100 ~ 3000; Described end-capping reagent is the derivative of the acid of C2 ~ C20 aliphatics list or the acid of C2 ~ C20 aliphatics list; Described an acidic catalyst is a kind of or several arbitrarily mixture in phosphoric acid, Hypophosporous Acid, 50, phosphorous acid and ortho phosphorous acid.
Further, described dimeracid is the dimeracid of C18 unsaturated aliphatic, derivative by linoleic acid dimer, dimerization oleic acid, dimerization linolenic acid, dimerization behenic acid, dimerization elaidic acid and dimerization eleostearic acid; Described polyether polyamine is a kind of or several arbitrarily mixture in the trade mark D-230, D-400, D-2000, T-403; Described C6 ~ C12 aliphatic dicarboxylic acid is a kind of or several arbitrarily mixture in suberic acid, nonane diacid, sebacic acid and dodecanedioic acid; Described C2 ~ C8 aliphatie diamine is a kind of or several arbitrarily mixture in quadrol, pentamethylene diamine and 2 methyl pentamethylenediamine; Described end-capping reagent is the acid of C12 ~ C20 aliphatics list.
Further, described C6 ~ C12 aliphatic dicarboxylic acid is sebacic acid; Described C2 ~ C8 aliphatie diamine is 2 methyl pentamethylenediamine; Described end-capping reagent is stearic acid.
The present invention also provides a kind of preparation method with the hot melt adhesive of pressure-sensitive, comprise the steps: at one with thermometer, mechanical stirrer, dimeracid is added in the reaction flask of prolong and nitrogen access tube, aliphatic dicarboxylic acid, end-capping reagent, polyetheramine and acid catalyst, then, aliphatie diamine is loaded in constant pressure addition pipe, pass into nitrogen anti-oxidant, stir heat temperature raising simultaneously, when the temperature in reaction flask reaches 130 DEG C, start to drip aliphatie diamine, drip in 1h, the temperature keeping reaction flask during dropping is 125-135 DEG C, if temperature is more than 140 DEG C, should stop or slowing down rate of addition, until aliphatie diamine is dripped, after dropping terminates, slowly temperature of reaction is raised according to the temperature rise rate of 20 DEG C/h, start slowly to be warming up to 240 DEG C, water is had to distillate in temperature-rise period, when temperature of reaction reaches 240 DEG C, keep this temperature section 1h, and the water distillated is reacted in metering, when reaching 90% of theoretical value, can start to carry out vacuumizing decompression with vacuum pump, vacuum tightness < 100Pa, keep stir speed (S.S.), whole polycondensation is completed under the state of high vacuum, remove vacuum after reaction 3h and terminate reaction, finally, be poured on zellon plate by the polyamide resin of melting, obtain yellow adhesive tape, at 50 DEG C, drying completes for 24 hours.
The invention has the beneficial effects as follows: the polyamide hot high temperature melt viscosity that the present invention has pressure-sensitive is higher, and snappiness is high, high to substrate bonding power, is applicable to process industry pressure-sensitive adhesive tape and sticker.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
145.70g C is added in a 500mL four-hole boiling flask with thermometer, agitator, prolong and nitrogen tube
16unsaturated aliphatic dimeracid, 5.10g sebacic acid, 23.20g polyetheramine D-230,58.00g polyetheramine D-2000,2.20gC
12the acid of aliphatics list, 0.20g ortho phosphorous acid, and 10.40g2-making methylpentamethylenediamine diamine is encased in constant pressure funnel, pass into nitrogen gas stirring and start heating, in 60 minutes, temperature is raised to 120 DEG C, and start slowly to drip 2 methyl pentamethylenediamine in this temperature, dropwise in 60 minutes, now temperature is raised to 130 DEG C, and salify 2 hours at this temperature, and then slowly heat up, have water in the process to steam, in 3 hours, temperature is raised to 240 DEG C, keep 5 hours at this temperature, then with vacuum pump evacuation 3 little up to pressure be 200Pa, last discharging under nitrogen protection, obtain light yellow adhesive tape.
Embodiment 2
113.60gC is added in a 500mL four-hole boiling flask with thermometer, agitator, prolong and nitrogen tube
18unsaturated aliphatic dimeracid, 23.10g suberic acid, 35.40g polyetheramine D-230,1.00gC
16the acid of aliphatics list, 0.20g phosphoric acid, and 11.20g2-making methylpentamethylenediamine diamine is encased in constant pressure funnel, pass into nitrogen gas stirring and start heating, in 60 minutes, temperature is raised to 120 DEG C, and start slowly to drip 2 methyl pentamethylenediamine in this temperature, dropwise in 60 minutes, now temperature is raised to 130 DEG C, and salify 2 hours at this temperature, and then slowly heat up, have water in the process to steam, in 3 hours, temperature is raised to 240 DEG C, keep 5 hours at this temperature, then with vacuum pump evacuation 3 little up to pressure be 200Pa, last discharging under nitrogen protection, obtain light yellow adhesive tape.
Embodiment 3
165.10gC is added in a 500mL four-hole boiling flask with thermometer, agitator, prolong and nitrogen tube
20unsaturated aliphatic dimeracid, 1.20g nonane diacid, 78.40g polyetheramine D-2000,1.40gC
20the acid of aliphatics list, 0.50g phosphorous acid, and 20.60g2-making methylpentamethylenediamine diamine is encased in constant pressure funnel, pass into nitrogen gas stirring and start heating, in 60 minutes, temperature is raised to 120 DEG C, and start slowly to drip 2 methyl pentamethylenediamine in this temperature, dropwise in 60 minutes, now temperature is raised to 130 DEG C, and salify 2 hours at this temperature, and then slowly heat up, have water in the process to steam, in 3 hours, temperature is raised to 240 DEG C, keep 5 hours at this temperature, then with vacuum pump evacuation 3 little up to pressure be 200Pa, last discharging under nitrogen protection, obtain light yellow adhesive tape.
Embodiment 4
At one with thermometer, agitator, 138.30g linoleic acid dimer is added in the 500mL four-hole boiling flask of prolong and nitrogen tube, 3.90g dodecanedioic acid, 15.20g polyetheramine D-230, 24.00g polyetheramine D-2000, 6.20g stearic acid, 0.20g Hypophosporous Acid, 50, and 8.50g2-making methylpentamethylenediamine diamine is encased in constant pressure funnel, pass into nitrogen gas stirring and start heating, in 60 minutes, temperature is raised to 120 DEG C, and start slowly to drip 2 methyl pentamethylenediamine in this temperature, dropwise in 60 minutes, now temperature is raised to 130 DEG C, and salify 2 hours at this temperature, and then slowly heat up, have water in the process to steam, in 3 hours, temperature is raised to 240 DEG C, keep 5 hours at this temperature, then with vacuum pump evacuation 3 little up to pressure be 200Pa, last discharging under nitrogen protection, obtain light yellow adhesive tape.
Embodiment 5
At one with thermometer, agitator, 127.70g dimerization behenic acid is added in the 500mL four-hole boiling flask of prolong and nitrogen tube, 13.20g sebacic acid, 2.20g polyetheramine T-403, 33.00g polyetheramine D-2000, 3.80g stearic acid, 0.20g ortho phosphorous acid, and 17.60g2-making methylpentamethylenediamine diamine is encased in constant pressure funnel, pass into nitrogen gas stirring and start heating, in 60 minutes, temperature is raised to 120 DEG C, and start slowly to drip 2 methyl pentamethylenediamine in this temperature, dropwise in 60 minutes, now temperature is raised to 130 DEG C, and salify 2 hours at this temperature, and then slowly heat up, have water in the process to steam, in 3 hours, temperature is raised to 240 DEG C, keep 5 hours at this temperature, then with vacuum pump evacuation 3 little up to pressure be 200Pa, last discharging under nitrogen protection, obtain light yellow adhesive tape.
Comparative example
This sample is conventional commercial polyacrylic ester hot melt adhesive sample, and its external appearance characteristic is: amber square solid.Put it in the baking oven of 150 DEG C, melted, completely to be melted, the sample of melting is poured on zellon plate, obtains amber blanket, test after dry 24 hours at 50 DEG C.
The sample obtained by embodiment 1-5 by the following method and the properties of comparative example have carried out contrast test:
Melt viscosity is tested: the melt viscosity adopting Brkfield DV-E type rotational viscosimeter test sample, take 10.0g polyamide hot sample, model is selected to be the rotor of S27 during test, temperature controls at 150 DEG C, and constantly regulate speed of rotation, make its test value be positioned at the linearity range of 10% ~ 90%, after stable, record observed value, viscosity unit: mPa.s, 150 DEG C.
Shore hardness is tested: according to ASTM D-2240-05 test.
Tensile strength and test of elongation rate: sample is made dumbbell shape according to according to standard A STM-D638-2003, carry out tensile property test after detect thickness, tensile strength unit: MPa; Elongation unit: %.
Shearing resistance is tested: according to standard A STM-D1002-72 sample preparation, material is Al, nylon66 and PBT, and overlap joint area is 12.5 × 25 (mm2), and cooling is placed on the performance test carrying out shearing resistance under test condition after 12h.Shearing resistance unit: MPa.
The properties of sample contrast test that embodiment 1 ~ 5 and comparative example obtain the results are shown in Table 1.
Table 1
As can be seen from Table 1, polyamide resin synthesized by the present invention has higher melt viscosity and snappiness, and to various substrate bonding power all higher than polyacrylic ester hot-fusible pressure-sensitive adhesive, so polyamide hot synthesized by the present invention prospect in the manufacture application of pressure-sensitive adhesive tape and sticker is better.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. one kind has the hot melt adhesive of pressure-sensitive, high temperature melt viscosity (150 DEG C) is 1500 ~ 15000mPas, shore hardness is 10 ~ 40, tensile strength is 0.1 ~ 1MPa, elongation at break is > 1000%, it is characterized in that: formed by the following composition polycondensation by mole percent: 30% ~ 45% dimeracid, 5% ~ 20% aliphatic dicarboxylic acid, 20% ~ 30% aliphatie diamine, 15% ~ 25% polyetheramine, 0.01% ~ 0.06% end-capping reagent and 0.01% ~ 0.1% acid catalyst, the mole number of described aliphatic dicarboxylic acid is less than or equal to 40% of dimeracid mole number.
2. a kind of hot melt adhesive with pressure-sensitive according to claim 1, is characterized in that: high temperature melt viscosity (150 DEG C) is 2000 ~ 13000 mPas; Shore hardness is 15 ~ 35; Tensile strength is 0.15 ~ 0.9MPa; Elongation at break is > 1500%; The molecular fraction of end-capping reagent is 0.01% ~ 0.02%, and the molecular fraction of acid catalyst is 0.05% ~ 0.1%; The mole number of described aliphatic dibasic acid is less than or equal to 35% of dimeracid mole number.
3. a kind of hot melt adhesive with pressure-sensitive according to claim 1, is characterized in that: in described dimeracid, mass fraction shared by tripolymer is 5% ~ 10%, mass fraction shared by dimer acids is 80% ~ 90%, mass fraction shared by monomer acids is 5% ~ 10%.
4. a kind of hot melt adhesive with pressure-sensitive according to claim 1, is characterized in that: described dimeracid is C
16~ C
20unsaturated aliphatic dimeracid; Described aliphatic dicarboxylic acid is C
6~ C
12aliphatic dicarboxylic acid; Described aliphatie diamine is C
2~ C
8aliphatie diamine or C
2~ C
8the derivative of aliphatie diamine; Described polyetheramine is for containing 2 ~ 3 Amino End Group, and molecular weight is the polyether polyamine of 100 ~ 3000; Described end-capping reagent is C
2~ C
20the acid of aliphatics list or C
2~ C
20the derivative of aliphatics list acid; Described an acidic catalyst is a kind of or several arbitrarily mixture in phosphoric acid, Hypophosporous Acid, 50, phosphorous acid and ortho phosphorous acid.
5. a kind of hot melt adhesive with pressure-sensitive according to claim 4, is characterized in that: described dimeracid is C
18the dimeracid of unsaturated aliphatic, derivative by linoleic acid dimer, dimerization oleic acid, dimerization linolenic acid, dimerization behenic acid, dimerization elaidic acid and dimerization eleostearic acid; Described polyether polyamine is a kind of or several arbitrarily mixture in the trade mark D-230, D-400, D-2000, T-403; Described C
6~ C
12aliphatic dicarboxylic acid is a kind of or several arbitrarily mixture in suberic acid, nonane diacid, sebacic acid and dodecanedioic acid; Described C
2~ C
8aliphatie diamine is a kind of or several arbitrarily mixture in quadrol, pentamethylene diamine and 2 methyl pentamethylenediamine; Described end-capping reagent is C
12~ C
20the acid of aliphatics list.
6. a kind of hot melt adhesive with pressure-sensitive according to claim 5, is characterized in that: described C
6~ C
12aliphatic dicarboxylic acid is sebacic acid; Described C
2~ C
8aliphatie diamine is 2 methyl pentamethylenediamine; Described end-capping reagent is stearic acid.
7. prepare a kind of preparation method with the hot melt adhesive of pressure-sensitive according to claim 1, comprise the steps: at one with thermometer, mechanical stirrer, dimeracid is added in the reaction flask of prolong and nitrogen access tube, aliphatic dicarboxylic acid, end-capping reagent, polyetheramine and acid catalyst, then, aliphatie diamine is loaded in constant pressure addition pipe, pass into nitrogen anti-oxidant, stir heat temperature raising simultaneously, when the temperature in reaction flask reaches 130 DEG C, start to drip aliphatie diamine, drip in 1h, the temperature keeping reaction flask during dropping is 125-135 DEG C, if temperature is more than 140 DEG C, should stop or slowing down rate of addition, until aliphatie diamine is dripped, after dropping terminates, slowly temperature of reaction is raised according to the temperature rise rate of 20 DEG C/h, start slowly to be warming up to 240 DEG C, water is had to distillate in temperature-rise period, when temperature of reaction reaches 240 DEG C, keep this temperature section 1h, and the water distillated is reacted in metering, when reaching 90% of theoretical value, can start to carry out vacuumizing decompression with vacuum pump, vacuum tightness < 100Pa, keep stir speed (S.S.), whole polycondensation is completed under the state of high vacuum, remove vacuum after reaction 3h and terminate reaction, finally, be poured on zellon plate by the polyamide resin of melting, obtain yellow adhesive tape, at 50 DEG C, drying completes for 24 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750330A (en) * | 2016-11-14 | 2017-05-31 | 烟台德邦科技有限公司 | A kind of preparation method of polyester amide hot melt adhesive |
| CN107418503A (en) * | 2017-08-24 | 2017-12-01 | 安徽省鸿鑫生物科技有限公司 | A kind of vehicle glass pad pasting light solidifying hot-melt adhesive and preparation method thereof |
| CN109605878A (en) * | 2018-12-17 | 2019-04-12 | 吕拴力 | A kind of fabrication polyamide adhesive material |
| CN109652004A (en) * | 2018-12-17 | 2019-04-19 | 天津海虹科技有限公司 | A kind of preparation method of fabrication polyamide binder |
| CN109652003A (en) * | 2018-12-17 | 2019-04-19 | 天津海虹科技有限公司 | A kind of fabrication polyamide binder |
| CN109679568A (en) * | 2018-12-07 | 2019-04-26 | 苏州市邦岑新材料股份有限公司 | A kind of water soluble polyamide hot melt adhesive |
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| US20130237654A1 (en) * | 2011-09-06 | 2013-09-12 | Flint Trading, Inc. | Anti-Foaming Agents for Hot-Melt Adhesives |
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| CN101928544A (en) * | 2010-09-21 | 2010-12-29 | 烟台德邦电子材料有限公司 | Polyamide hot cement with high softening point and low-temperature resistance, and preparing method thereof |
| US20130237654A1 (en) * | 2011-09-06 | 2013-09-12 | Flint Trading, Inc. | Anti-Foaming Agents for Hot-Melt Adhesives |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750330A (en) * | 2016-11-14 | 2017-05-31 | 烟台德邦科技有限公司 | A kind of preparation method of polyester amide hot melt adhesive |
| CN107418503A (en) * | 2017-08-24 | 2017-12-01 | 安徽省鸿鑫生物科技有限公司 | A kind of vehicle glass pad pasting light solidifying hot-melt adhesive and preparation method thereof |
| CN109679568A (en) * | 2018-12-07 | 2019-04-26 | 苏州市邦岑新材料股份有限公司 | A kind of water soluble polyamide hot melt adhesive |
| CN109605878A (en) * | 2018-12-17 | 2019-04-12 | 吕拴力 | A kind of fabrication polyamide adhesive material |
| CN109652004A (en) * | 2018-12-17 | 2019-04-19 | 天津海虹科技有限公司 | A kind of preparation method of fabrication polyamide binder |
| CN109652003A (en) * | 2018-12-17 | 2019-04-19 | 天津海虹科技有限公司 | A kind of fabrication polyamide binder |
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