CN108822783A - A kind of preparation method of copolyester hot melt adhesive - Google Patents
A kind of preparation method of copolyester hot melt adhesive Download PDFInfo
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- CN108822783A CN108822783A CN201810472530.4A CN201810472530A CN108822783A CN 108822783 A CN108822783 A CN 108822783A CN 201810472530 A CN201810472530 A CN 201810472530A CN 108822783 A CN108822783 A CN 108822783A
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- acid
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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
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
- C09J167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Artificial Filaments (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of preparation method of copolyesters hot melt, especially a kind of preparation method suitable for spinning the copolyester hot melt adhesive of meldable fibre.The present invention has mainly picked up specific material and proportion design, especially after esterification and polycondensation reaction, in-lubricant, nucleating agent and the thermoplastic polyurethane for continuing to put into special ratios in the reaction product are blended again, multiple performance indicators such as open hour, elasticity modulus, molding shrinkage, the elongation at break of final copolyester hot melt adhesive product are balanced, it is made to meet spinnability and the requirement convenient for construction.
Description
Technical field
The present invention relates to a kind of preparation method of copolyesters hot melt, especially a kind of copolyesters suitable for spinning meldable fibre
The preparation method of hot melt adhesive.
Background technique
As environmental issue is of increasing concern, the application field for not needing the hot melt adhesion material of solvent is also more and more richer
It is rich.Meldable fibre is a kind of hot melt adhesion material being concerned in recent years, in application, its is blended in fabric or vamp,
It is melted after process using low temperature pressing, the general fibre near it is bonded together, played the role of bonding sizing, subtract
Lack the process using substrate, has made final products more lightweight, it is also more convenient in production.
Currently, the substrate of the most common meldable fibre is copolyamide hot melt adhesive on the market, but its cost is generally higher, and
There are problems that sizing demoulding time is longer and is easy to happen phenol xanthochromia.Conventional copolyester hot melt adhesive advantage of lower cost, but
Its fusing point is generally greater than copolyamide hot melt adhesive, can not play the role of bonding sizing at relatively low temperature, and other performances refer to
Mark aspect can not also fully meet the requirement of spinnability.
Therefore the copolyester hot melt adhesive for being suitable for spinning meldable fibre how is prepared, become problem to be solved.
Summary of the invention
It is an object of the invention to solve above-mentioned technical problem, a kind of preparation method of copolyester hot melt adhesive is proposed, so that
Resulting copolyester hot melt adhesive is prepared through the invention, is very suitable for being spun into meldable fibre.
The technical scheme adopted by the invention is as follows：A kind of preparation method of copolyester hot melt adhesive, includes the following steps：
（1）The binary acid that will be made of terephthalic acid (TPA), M-phthalic acid and other aliphatic diacids, by butanediol and other rouge
The dihydric alcohol and catalyst of fat race glycol composition are added in reaction kettle by a preset ratio and are started esterification, are reacted
Initial temperature is 160 DEG C, is gradually warming up to 210 DEG C, when water yield reaches 95% or more of theoretical value, Esterification Stage terminates；
（2）Antioxidant is put into the product of esterification, progress polycondensation reaction, within the scope of 240 DEG C ~ 250 DEG C of reaction temperature,
It vacuumizes and ensures reacting kettle inner pressure 50Pa ~ 100Pa, the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and in-lubricant, nucleating agent and thermoplastic polyurethane is added, and keeps system temperature 230 DEG C ~ 250
DEG C, 1h is stirred, system discharges after mixing.
Above-mentioned steps（1）In, other aliphatic diacids are selected from adipic acid, decanedioic acid, dodecanedioic acid or tridecandioic acid
One of；Other aliphatic diols are selected from one of hexylene glycol, diethylene glycol (DEG), ethylene glycol or neopentyl glycol；Catalyst is titanium
Sour four butyl esters；Meanwhile each material proportion is：
Binary acid：The molar ratio of dihydric alcohol is 1:1.5；
In binary acid, terephthalic acid (TPA)：M-phthalic acid：The molar ratio of other aliphatic diacids is 1:0.8~1.2:0.1~0.2；
In dihydric alcohol, butanediol：The molar ratio of other aliphatic diols is 1:0.4~0.8；
The additional amount of catalyst is the 0.02% ~ 0.05% of binary acid and dihydric alcohol gross mass.
Above-mentioned steps（2）In, the trade mark of antioxidant is 1010, and additional amount is binary acid and dihydric alcohol gross mass
0.25%~0.75%。
Above-mentioned steps（3）In, in-lubricant is selected from ethylene bis stearamide, erucyl amide, oleamide or oleoyl ethyl alcohol
One of amine, additional amount are the 0.5% ~ 1.5% of binary acid and dihydric alcohol gross mass；Nucleating agent be selected from mica powder, talcum powder,
One of calcium carbonate or fumed silica, additional amount are the 0.5% ~ 1% of binary acid and dihydric alcohol gross mass；Above-mentioned thermoplastic
Property polyurethane additional amount be the 10% ~ 30% of binary acid and dihydric alcohol gross mass, the trade mark is preferably TPU 301 or TPU 302.
Innovation of the invention is, has picked up specific material and proportion design, especially anti-in esterification and polycondensation
After answering, in-lubricant, nucleating agent and the thermoplastic polyurethane for continuing to put into special ratios in the reaction product are total to again
It is mixed, balance multiple property such as open hour, elasticity modulus, molding shrinkage, elongation at break of final copolyester hot melt adhesive product
Energy index, makes it meet spinnability and the requirement convenient for construction.The beneficial effects of the present invention are prepare gained through the invention
Copolyester hot melt adhesive, be provided simultaneously with the spies such as fusing point is lower, elasticity modulus is higher, molding shrinkage is lower, the open hour are shorter
Property, it is very suitable for being spun into meldable fibre, meets related industry application demand.
Specific embodiment
The present invention is addressed further under below by embodiment, but is not limited thereto.
Embodiment 1：
A kind of preparation method of copolyester hot melt adhesive, preparation step are as follows：
（1）The binary acid that will be made of terephthalic acid (TPA) 132.8g, M-phthalic acid 106.24g and adipic acid 23.36g, and by
The dihydric alcohol and catalyst butyl titanate 0.10g of butanediol 154.29g and hexylene glycol 80.91g composition, are added to reaction
In kettle, esterification is carried out, reacting initial temperature is 160 DEG C, 210 DEG C is gradually warming up to, when water yield reaches the 95% of theoretical value
Or more when, Esterification Stage terminates；
（2）The antioxidant 1.24g that the trade mark is 1010 is added in esterification products, starts to carry out polycondensation reaction, reaction temperature control
System vacuumizes within the scope of 240 DEG C ~ 250 DEG C and ensures reacting kettle inner pressure 50Pa ~ 100Pa, and the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and the heat that ethylene bis stearamide 7.46g, mica powder 4.98g and the trade mark are TPU301 is added
Plastic polyurethane 49.76g is kept for 230 DEG C ~ 250 DEG C of system temperature, stirs 1h, and system discharges after mixing.
A1 is labeled as by 1 products therefrom sample of embodiment.
Embodiment 2：
A kind of preparation method of copolyester hot melt adhesive, preparation step are as follows：
（1）The binary acid that will be made of terephthalic acid (TPA) 116.2g, M-phthalic acid 139.44g and decanedioic acid 14.14g, and by
The dihydric alcohol and catalyst butyl titanate 0.25g of butanediol 120.75g and diethylene glycol (DEG) 113.77g composition, are added to reaction
In kettle, esterification is carried out, reacting initial temperature is 160 DEG C, 210 DEG C is gradually warming up to, when water yield reaches the 95% of theoretical value
Or more when, Esterification Stage terminates；
（2）The antioxidant 3.78g that the trade mark is 1010 is added in esterification products, starts to carry out polycondensation reaction, reaction temperature control
System vacuumizes within the scope of 240 DEG C ~ 250 DEG C and ensures reacting kettle inner pressure 50Pa ~ 100Pa, and the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and the thermoplastic poly that erucyl amide 2.52g, talcum powder 2.52g and the trade mark are TPU302 is added
Urethane 151.29g is kept for 230 DEG C ~ 250 DEG C of system temperature, stirs 1h, and system discharges after mixing.
A2 is labeled as by 2 products therefrom sample of embodiment.
Embodiment 3：
A kind of preparation method of copolyester hot melt adhesive, preparation step are as follows：
（1）The binary acid that will be made of terephthalic acid (TPA) 141,1g, M-phthalic acid 112.88g and dodecanedioic acid 39.1g, and
The dihydric alcohol and catalyst butyl titanate 0.10g being made of butanediol 163.93g and ethylene glycol 45.17g are added to anti-
It answers in kettle, carries out esterification, reacting initial temperature is 160 DEG C, 210 DEG C is gradually warming up to, when water yield reaches theoretical value
When 95% or more, Esterification Stage terminates；
（2）The antioxidant 1.26g that the trade mark is 1010 is added in esterification products, starts to carry out polycondensation reaction, reaction temperature control
System vacuumizes within the scope of 240 DEG C ~ 250 DEG C and ensures reacting kettle inner pressure 50Pa ~ 100Pa, and the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and the thermoplastic poly that oleamide 7.53g, calcium carbonate 5.02g and the trade mark are TPU301 is added
Urethane 150.65g is kept for 230 DEG C ~ 250 DEG C of system temperature, stirs 1h, and system discharges after mixing.
A3 is labeled as by 3 products therefrom sample of embodiment.
Embodiment 4：
A kind of preparation method of copolyester hot melt adhesive, preparation step are as follows：
（1）The binary acid that will be made of terephthalic acid (TPA) 116.2g, M-phthalic acid 139.44g and tridecandioic acid 17.08g,
Dihydric alcohol and catalyst butyl titanate 0.25g with being made of butanediol 120.75g and neopentyl glycol 111.63g, are added
Into reaction kettle, esterification is carried out, reacting initial temperature is 160 DEG C, 210 DEG C is gradually warming up to, when water yield reaches theoretical
Value 95% or more when, Esterification Stage terminates；
（2）The antioxidant 3.79g that the trade mark is 1010 is added in esterification products, starts to carry out polycondensation reaction, reaction temperature control
System vacuumizes within the scope of 240 DEG C ~ 250 DEG C and ensures reacting kettle inner pressure 50Pa ~ 100Pa, and the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and it is TPU302's that Oleoyl monoethanolamide 2.52g, meteorology silica 2.52g and the trade mark, which is added,
Thermoplastic polyurethane 50.51g is kept for 230 DEG C ~ 250 DEG C of system temperature, stirs 1h, and system discharges after mixing.
A4 is labeled as by 4 products therefrom sample of embodiment.
By the various embodiments described above products obtained therefrom, commercially available normal polyester hot melt adhesive and commercially available routine can spinning copolyamide heat
The correlated performance of melten gel is tested, as a result as shown in table 1 below.
Wherein, fusing point testing standard refers to GB/T19466-2004；Inherent viscosity testing standard refers to GB/T2794-
1995；Molding shrinkage testing standard refers to GB/T 15585-1995；Open hour testing standard refers to HG/T3716-2003；
Tensile modulus of elasticity and elongation at break testing standard refer to GB/T 1040.1-2006；Potential phenol xanthochromia series testing standard ginseng
Examine GB/T 29778-2013.
Table 1：Performance test deck watch
| Index | A1 | A2 | A3 | A4 | Commercially available standard copolymerization ester hot melt adhesive | Commercially available routine can spinning copolyamide hot melt adhesive |
| Fusing point（℃） | 125 | 122 | 120 | 123 | 130 | 125 |
| Inherent viscosity | 0.75 | 0.68 | 0.73 | 0.70 | 0.6 | 0.65 |
| Molding shrinkage | 1.2% | 0.8% | 0.6% | 0.7% | 2.8% | 1.6% |
| Open hour | 1’30” | 1’40” | 1’45” | 1’40” | 3’00” | 2’30” |
| Tensile modulus of elasticity (GPa) | 140 | 150 | 130 | 140 | 80 | 120 |
| Elongation at break | 210 | 220 | 235 | 215 | 120 | 165 |
| Potential phenol xanthochromia series | 5 | 4-5 | 5 | 4-5 | 5 | 2 |
It will be evident that resulting copolyester hot melt adhesive is prepared through the invention, in fusing point and inherent viscosity side from upper table 1
Face, with standard copolymerization ester hot melt adhesive and it is conventional can spinning copolyamide hot melt adhesive difference it is little, it is same convenient for sizing；But its
Comprehensive performance in terms of molding shrinkage, open hour, tensile modulus of elasticity, elongation at break and phenol xanthochromia series, then have bright
Aobvious promotion.Resulting copolyester hot melt adhesive is prepared through the invention, molding shrinkage significantly reduces, and the open hour shorten,
Tensile modulus of elasticity increases, and elongation at break increases, when being spun into meldable fibre, the problems such as being not in fracture of wire, haircuts；And compared with
Commercially available routine can be for spinning copolyamide, and phenol xanthochromia technology is obviously improved, and is more suitable for downstream industry application.
Claims (5)
1. a kind of preparation method of copolyester hot melt adhesive, which is characterized in that include the following steps：
（1）The binary acid that will be made of terephthalic acid (TPA), M-phthalic acid and other aliphatic diacids, by butanediol and other rouge
The dihydric alcohol and catalyst of fat race glycol composition are added in reaction kettle by a preset ratio and are started esterification, are reacted
Initial temperature is 160 DEG C, is gradually warming up to 210 DEG C, when water yield reaches 95% or more of theoretical value, Esterification Stage terminates；
（2）Antioxidant is put into the product of esterification, progress polycondensation reaction, within the scope of 240 DEG C ~ 250 DEG C of reaction temperature,
It vacuumizes and ensures reacting kettle inner pressure 50Pa ~ 100Pa, the 2h aftercondensated stage terminates；
（3）Logical nitrogen releases vacuum, and in-lubricant, nucleating agent and thermoplastic polyurethane is added, and keeps system temperature 230 DEG C ~ 250
DEG C, 1h is stirred, system discharges after mixing；
The step（1）In, each material proportion is：
In binary acid, terephthalic acid (TPA)：M-phthalic acid：The molar ratio of other aliphatic diacids is 1:0.8~1.2:0.1~0.2；
In dihydric alcohol, butanediol：The molar ratio of other aliphatic diols is 1:0.4~0.8；
Binary acid：The molar ratio of dihydric alcohol is 1:1.5；
The step（3）In, in-lubricant is in ethylene bis stearamide, erucyl amide, oleamide or Oleoyl monoethanolamide
One kind, additional amount is the 0.5% ~ 1.5% of binary acid and dihydric alcohol gross mass；Nucleating agent is selected from mica powder, talcum powder, carbonic acid
One of calcium or fumed silica, additional amount are the 0.5% ~ 1% of binary acid and dihydric alcohol gross mass；Thermoplastic polyurethane
Additional amount be the 10% ~ 30% of binary acid and dihydric alcohol gross mass.
2. the preparation method of copolyesters hot melt as described in claim 1, which is characterized in that the step（1）In, other fat
Race's diacid is selected from one of adipic acid, decanedioic acid, dodecanedioic acid or tridecandioic acid；Other aliphatic diols select oneself two
One of alcohol, diethylene glycol (DEG), ethylene glycol or neopentyl glycol.
3. the preparation method of copolyesters hot melt as described in claim 1, which is characterized in that the step（1）In, catalyst is
Butyl titanate, additional amount are the 0.02% ~ 0.05% of binary acid and dihydric alcohol gross mass.
4. the preparation method of copolyesters hot melt as described in claim 1, which is characterized in that the step（2）In, antioxidant
The trade mark is 1010, and additional amount is the 0.25% ~ 0.75% of binary acid and dihydric alcohol gross mass.
5. the preparation method of copolyesters hot melt as described in claim 1, which is characterized in that above-mentioned steps（3）In, thermoplastic poly
The trade mark of urethane is TPU 301 or TPU 302.
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| CN201810472530.4A CN108822783A (en) | 2018-05-17 | 2018-05-17 | A kind of preparation method of copolyester hot melt adhesive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787809A (en) * | 2021-07-30 | 2021-12-14 | 泉州辉丽鞋服有限公司 | Pre-laminating process of microfiber leather and hot melt adhesive film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787809A (en) * | 2021-07-30 | 2021-12-14 | 泉州辉丽鞋服有限公司 | Pre-laminating process of microfiber leather and hot melt adhesive film |
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