CN102408867B - Process for preparing high temperature-resistant polyester hot melt adhesive powder - Google Patents
Process for preparing high temperature-resistant polyester hot melt adhesive powder Download PDFInfo
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- CN102408867B CN102408867B CN 201110268979 CN201110268979A CN102408867B CN 102408867 B CN102408867 B CN 102408867B CN 201110268979 CN201110268979 CN 201110268979 CN 201110268979 A CN201110268979 A CN 201110268979A CN 102408867 B CN102408867 B CN 102408867B
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- high temperature
- melt adhesive
- polyester hot
- hot melt
- temperature resistance
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Abstract
The invention discloses a process for preparing high temperature-resistant polyester hot melt adhesive powder, comprising the following steps of: firstly adding colloidal particles composed of polyester and polyamide in a weight ratio of 3: 1 to a reaction kettle, and then adding a catalyst accounting for 0.1% of the total weight of the colloidal particles and an antioxidant accounting for 0.01% of the total weight of the colloidal particles to the reaction kettle; heating the kettle under protection by nitrogen until the colloidal particles are molten, starting stirring, increasing the temperature to a range of 240-250 DEG C, keeping this state for 3-6 hours and performing copolymerization; next, reducing the pressure until the viscosity of the melt reaches 77.3 Pa.s, removing low molecular materials having the molecular weight less than 1000 in the copolymerization system; after the viscosity of the melt reaches 77.3 Pa.s, introducing nitrogen to the normal pressure at first and then changing the pressure to 1.08 barometric pressures; pressing the melt material into a water tank in form of strips, and performing grain-sized dicing after cooling, thereby obtaining the high temperature-resistant polyester hot melt adhesive particles; and finally, crushing the high temperature-resistant polyester hot melt adhesive particles and sieving the particles using a 200-mesh sieve, thus obtaining the high temperature-resistant polyester hot melt adhesive powder. The product of the process of the invention is high in bonding strength, convenient to control hot pressing temperatures, resistant to either dry cleaning or water washing, and suitable for bonding various fabrics.
Description
[technical field]
The present invention relates to field of fine chemical, relate in particular to the preparation technology of high temperature resistance polyester hot-melt adhesive powder.
[background technology]
Polyester hot-melt adhesive is widely used on the Pading cloth, and common polyester hot-melt adhesive is 70-100 ℃ of tendency that softening temperature is arranged and flow, and bonding strength is lower, can not use under higher temperature.The molecular weight that increases resin can improve softening temperature and yield temperature, but can cause viscosity to increase severely, and is unfavorable for that coat operations and tackiness agent are difficult to soak into adherend, and bonding strength is poor.
And in the crushing process of micelle, conventional at present solvent precipitation and the pollution of deep cooling comminuting method weighs, cost is high.
[summary of the invention]
Purpose of the present invention solves the problems of the prior art exactly, proposes a kind of preparation technology of high temperature resistance polyester hot-melt adhesive powder, can be not softening in the following temperature of fusing point, the a little higher than fusing point of temperature is fusing immediately just, be convenient to coat operations, bonding strength is good, is applicable to the bonding of various fabrics.
For achieving the above object; the present invention proposes a kind of preparation technology of high temperature resistance polyester hot-melt adhesive powder; to be that the micelle that 3: 1 polyester and polymeric amide are formed adds in the reactor by weight ratio earlier; 0.01% the oxidation inhibitor that in reactor, adds 0.1% catalyzer of micelle gross weight and micelle gross weight again; under nitrogen protection, be heated to the micelle fusing; start stirring; be warming up to 240～250 ℃; kept 3～6 hours; carry out copolyreaction; be decompressed to melt viscosity then and reach 77.3Pa.s; get rid of molecular weight in the copolymerization system less than 1000 low-molecular material; after reaching 77.3Pa.s to melt viscosity; inflated with nitrogen arrives first normal pressure, and then becomes 1.08 normal atmosphere, and melt material is pressed in the tank with strip; pelletizing obtains the high temperature resistance polyester hot melt adhesive tablet after cooling off, and sieves through 200 purpose screen clothes after the high temperature resistance polyester hot melt adhesive tablet being pulverized again and obtains the high temperature resistance polyester hot-melt adhesive powder.
As preferably, also be added with 5～6% diamine of micelle gross weight in the described reactor.
As preferably, described diamine adopts at least a in quadrol, hexanediamine, the propylene diamine.
As preferably, described catalyzer adopts acetate, and oxidation inhibitor adopts phosphorous acid ester.
As preferably, described acetate adopts at least a in zinc acetate, manganese acetate, sodium-acetate, ammonium acetate, Potassium ethanoate, the calcium acetate.
As preferably, the described high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow pulverizer to pulverize by normal temperature turbulent flow comminuting method.
As preferably, described turbulent flow pulverizer is made up of motor, positive and negative impeller and crushing chamber, the positive and negative impeller of electric motor driving rotates in the crushing chamber high speed, make to produce the eddy flow field of turbulent flow between the positive and negative impeller, the high temperature resistance polyester hot melt adhesive tablet impacts mutually, collides, shears and pulverized at eddy flow field of turbulent flow high frequency.
Beneficial effect of the present invention: the present invention adopts a step mass polymerization to utilize the polymeric amide co-polymerization modified polyester, owing to can form hydrogen bond between the macromolecular chain of polymeric amide, these hydrogen bonds occur between the macromolecular amido linkage, because the influence of intermolecular hydrogen bonding, it is narrow that polymeric amide has fusion range, softening under fusing point, the characteristics that a little higher than fusing point of temperature just melts immediately.Add polymeric amide and carry out copolymerization in the production process of polyester, can obtain the hot melt adhesive that fusion range is narrow, softening temperature is high, the product bonding strength is big, presses boiling hot temperature to control well, and not only anti-dry-cleaning but also water-fastness is applicable to the bonding of various fabrics.And this processing method has avoided solvent recuperation and product to purify, and technology is simple, stable, realizes greenization production.
Feature of the present invention and advantage will be elaborated by embodiment.
[embodiment]
The preparation technology of high temperature resistance polyester hot-melt adhesive powder; to be that the micelle that 3: 1 polyester and polymeric amide are formed adds in the reactor by weight ratio earlier; 0.01% the oxidation inhibitor that in reactor, adds 0.1% catalyzer of micelle gross weight and micelle gross weight again; under nitrogen protection, be heated to the micelle fusing; start stirring; be warming up to 240～250 ℃; kept 3～6 hours; carry out copolyreaction; be decompressed to melt viscosity then and reach 77.3Pa.s; get rid of molecular weight in the copolymerization system less than 1000 low-molecular material; after reaching 77.3Pa.s to melt viscosity; inflated with nitrogen arrives first normal pressure; and then become 1.08 normal atmosphere; change to malleation from normal pressure; improve temperature and vacuum tightness gradually and be conducive to the carrying out that reacts and the viscosity that increases characteristic; melt material is pressed in the tank with strip; pelletizing obtains the high temperature resistance polyester hot melt adhesive tablet after cooling off; sieve through the screen cloth of 200 orders (the powder process fineness reaches 75 μ m) after again the high temperature resistance polyester hot melt adhesive tablet being pulverized and obtain the high temperature resistance polyester hot-melt adhesive powder, during use the fusion of high temperature resistance polyester hot-melt adhesive powder just can be obtained the high temperature resistance polyester hot melt adhesive of excellent performance.
Described catalyzer adopts acetate, and acetate can adopt at least a in zinc acetate, manganese acetate, sodium-acetate, ammonium acetate, Potassium ethanoate, the calcium acetate.Oxidation inhibitor adopts phosphorous acid ester, can adopt the nontoxic phosphorous acid ester of PT-1500 of Nantong Ai Dewang chemical industry company limited, and its chemical name is the nontoxic phosphorous acid ester of PT-1500.
Also be added with 5～6% diamine of micelle gross weight in the described reactor, described diamine adopts at least a in quadrol, hexanediamine, the propylene diamine.The applicant finds that in modification by copolymerization reaction of the present invention the speed of speed of response depends on ester bond largely, and (CO-O-) speed of separating from terylene type polyester, general normal reaction time control was at 3-4 hour.But long reaction time has further increased cost like this, and there is the not good situation of stability in the product of production.Therefore, add diamine, can accelerate scission of link and the chain exchange of polyester molecule, to reduce to 1-2 hour the reaction times, enhance productivity, be switched " off " owing to the polyester macromolecule chain simultaneously, it is more even to make that ester bond and amido linkage distribute at macromolecular chain, and product performance further promote.
The described high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow pulverizer to pulverize by normal temperature turbulent flow comminuting method.Described turbulent flow pulverizer is made up of motor, positive and negative impeller and crushing chamber, the positive and negative impeller of electric motor driving rotates in the crushing chamber high speed, make to produce high energy swirling eddy field of turbulent flow (being called for short the eddy flow field of turbulent flow) between positive impeller and the anti-impeller, material particles impacts mutually, collides, shears and pulverized at eddy flow field of turbulent flow high frequency.Utilize the fast characteristic of field of turbulent flow heat transfer rate, the a large amount of heats that produce in pulverizing are taken out of outside the chamber by air-flow and powder, so can accomplish under the situation that does not need water-cooled, to carry out at normal temperatures the pulverizing of micelle, and can reach same equal yield line and the fineness of deep cooling grinding and processing.This technology has been exempted the use of chemical assistant, and environmental protection and energy saving have reduced product cost.
Above-described embodiment is to explanation of the present invention, is not limitation of the invention, any scheme after the simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (2)
1. the preparation technology of high temperature resistance polyester hot-melt adhesive powder; it is characterized in that: will be that the polyester of 3:1 and micelle that polymeric amide is formed add in the reactor by weight ratio earlier; 0.01% the oxidation inhibitor that in reactor, adds 0.1% catalyzer of micelle gross weight and micelle gross weight again; under nitrogen protection, be heated to the micelle fusing; start stirring; be warming up to 240～250 ℃; kept 3～6 hours; carry out copolyreaction; be decompressed to melt viscosity then and reach 77.3Pa.s; get rid of molecular weight in the copolymerization system less than 1000 low-molecular material; after reaching 77.3Pa.s to melt viscosity; inflated with nitrogen arrives first normal pressure; and then become 1.08 normal atmosphere; melt material is pressed in the tank with strip; pelletizing obtains the high temperature resistance polyester hot melt adhesive tablet after cooling off; sieve through 200 purpose screen clothes after again the high temperature resistance polyester hot melt adhesive tablet being pulverized and obtain the high temperature resistance polyester hot-melt adhesive powder; also be added with 5～6% diamine of micelle gross weight in the described reactor; described diamine adopts quadrol; hexanediamine; at least a in the propylene diamine; described catalyzer adopts acetate; oxidation inhibitor adopts phosphorous acid ester; described acetate adopts zinc acetate; manganese acetate; sodium-acetate; ammonium acetate; Potassium ethanoate; at least a in the calcium acetate, the described high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow pulverizer to pulverize by normal temperature turbulent flow comminuting method.
2. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 1, it is characterized in that: described turbulent flow pulverizer is made up of motor, positive and negative impeller and crushing chamber, the positive and negative impeller of electric motor driving rotates in the crushing chamber high speed, make to produce the eddy flow field of turbulent flow between the positive and negative impeller, the high temperature resistance polyester hot melt adhesive tablet impacts mutually, collides, shears and pulverized at eddy flow field of turbulent flow high frequency.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110268979 CN102408867B (en) | 2011-09-13 | 2011-09-13 | Process for preparing high temperature-resistant polyester hot melt adhesive powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110268979 CN102408867B (en) | 2011-09-13 | 2011-09-13 | Process for preparing high temperature-resistant polyester hot melt adhesive powder |
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| CN102408867A CN102408867A (en) | 2012-04-11 |
| CN102408867B true CN102408867B (en) | 2013-08-21 |
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| CN102960913B (en) * | 2012-12-18 | 2014-11-19 | 金华冠华水晶有限公司 | Making process of artificial crystal diamond adhesive powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4254254A (en) * | 1980-01-21 | 1981-03-03 | Eastman Kodak Company | Polyester amide fabric adhesives |
| CN1044664A (en) * | 1989-02-01 | 1990-08-15 | 河北工学院 | The manufacture method of polyesteramide thermosol for fabric |
| CN101586015A (en) * | 2009-06-15 | 2009-11-25 | 陈国新 | Method of producing polyester amide hot melt adhesive |
-
2011
- 2011-09-13 CN CN 201110268979 patent/CN102408867B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4254254A (en) * | 1980-01-21 | 1981-03-03 | Eastman Kodak Company | Polyester amide fabric adhesives |
| CN1044664A (en) * | 1989-02-01 | 1990-08-15 | 河北工学院 | The manufacture method of polyesteramide thermosol for fabric |
| CN101586015A (en) * | 2009-06-15 | 2009-11-25 | 陈国新 | Method of producing polyester amide hot melt adhesive |
Non-Patent Citations (4)
| Title |
|---|
| 王润珩等.织物用聚酯酰胺热熔胶的研制.《河北工学院学报》.1991,第20卷(第1期),第25-29页. |
| 王琛等.高分子材料改性技术.《高分子材料改性技术》.中国纺织出版社,2007,(第1版),第308、309页. * |
| 织物用聚酯酰胺热熔胶的研制;王润珩等;《河北工学院学报》;19910331;第20卷(第1期);第25-29页 * |
| 陈衍夏等.《纤维材料改性》.《纤维材料改性》.中国纺织出版社,2009,(第1版),第232页. * |
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