CN102408867A - 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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- CN102408867A CN102408867A CN2011102689797A CN201110268979A CN102408867A CN 102408867 A CN102408867 A CN 102408867A CN 2011102689797 A CN2011102689797 A CN 2011102689797A CN 201110268979 A CN201110268979 A CN 201110268979A CN 102408867 A CN102408867 A CN 102408867A
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- high temperature
- melt adhesive
- polyester hot
- temperature resistance
- resistance polyester
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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 has softening temperature and mobile tendency at 70-100 ℃, and bonding strength is lower, can not under higher temperature, use.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 weigh, cost is high.
[summary of the invention]
The object of the 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.
Be realizing above-mentioned purpose, the present invention proposes a kind of preparation technology of high temperature resistance polyester hot-melt adhesive powder, will be in the micelle adding reaction kettle formed of 3: 1 polyester and polymeric amide by weight ratio earlier; 0.01% of 0.1% of adding micelle gross weight catalyzer and micelle gross weight oxidation inhibitor in reaction kettle is heated to the micelle fusing under nitrogen protection again, starts 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, reach 77.3Pa.s to melt viscosity after, inflated with nitrogen arrives first normal pressure; And then become 1.08 normal atmosphere; Melt material is pressed in the tank with strip, and pelletizing obtains the high temperature resistance polyester hot melt adhesive tablet through cooling back, obtains the high temperature resistance polyester hot-melt adhesive powder with sieving through 200 purpose screen clothes after the pulverizing of high temperature resistance polyester hot melt adhesive tablet again.
As preferably, also be added with 5～6% diamine of micelle gross weight in the said reaction kettle.
As preferably, said diamine adopts at least a in quadrol, hexanediamine, the tn.
As preferably, said catalyzer adopts acetate, and oxidation inhibitor adopts phosphorous acid ester.
As preferably, said acetate adopts at least a in zinc acetate, manganese acetate, sodium-acetate, ammonium acetate, Potassium ethanoate, the calcium acetate.
As preferably, the said high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow kibbler to pulverize through normal temperature turbulent flow comminuting method.
As preferably; Said turbulent flow kibbler 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 ydrogen 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.In the production process of polyester, add polymeric amide and carry out copolymerization, 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-fast washing are applicable to the bonding of various fabrics.And this process method has avoided solvent recuperation and product to purify, and technology is simple, stable, realizes greenization production.
Characteristic of the present invention and advantage will be elaborated through embodiment.
[embodiment]
The preparation technology of high temperature resistance polyester hot-melt adhesive powder will be that the micelle that 3: 1 polyester and polymeric amide formed adds in the reaction kettle by weight ratio earlier, in reaction kettle, add 0.01% oxidation inhibitor of 0.1% catalyzer and the micelle gross weight of 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, and carried 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; Change to malleation from normal pressure; Improve temperature and vacuum tightness gradually and help 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; 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.
Said 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 ltd, 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 said reaction kettle, said diamine adopts at least a in quadrol, hexanediamine, the tn.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-) from the isolating speed of terylene type polyester, the general normal reaction time was controlled 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 quicken the 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 on macromolecular chain, and product performance further promote.
The said high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow kibbler to pulverize through normal temperature turbulent flow comminuting method.Said turbulent flow kibbler 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; Take a large amount of heats that produce in pulverizing outside the chamber out of 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 the 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.
The foregoing description is to explanation of the present invention, is not to qualification of the present invention, any scheme after the simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (7)
1. the preparation technology of high temperature resistance polyester hot-melt adhesive powder is characterized in that: will be that the micelle that 3: 1 polyester and polymeric amide formed adds in the reaction kettle by weight ratio earlier, and in reaction kettle, add 0.01% oxidation inhibitor of 0.1% catalyzer and the micelle gross weight of 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 through cooling back, obtains the high temperature resistance polyester hot-melt adhesive powder with sieving through 200 purpose screen clothes after the pulverizing of high temperature resistance polyester hot melt adhesive tablet again.
2. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 1 is characterized in that: 5～6% the diamine that also is added with the micelle gross weight in the said reaction kettle.
3. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 2 is characterized in that: said diamine adopts at least a in quadrol, hexanediamine, the tn.
4. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 3 is characterized in that: said catalyzer adopts acetate, and oxidation inhibitor adopts phosphorous acid ester.
5. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 4 is characterized in that: said acetate adopts at least a in zinc acetate, manganese acetate, sodium-acetate, ammonium acetate, Potassium ethanoate, the calcium acetate.
6. like the preparation technology of each described high temperature resistance polyester hot-melt adhesive powder in the claim 1～5, it is characterized in that: the said high temperature resistance polyester hot melt adhesive tablet is pulverized is to adopt the turbulent flow kibbler to pulverize through normal temperature turbulent flow comminuting method.
7. the preparation technology of high temperature resistance polyester hot-melt adhesive powder as claimed in claim 6; It is characterized in that: said turbulent flow kibbler 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.
Priority Applications (1)
| 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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| 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 true CN102408867A (en) | 2012-04-11 |
| CN102408867B CN102408867B (en) | 2013-08-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102960913A (en) * | 2012-12-18 | 2013-03-13 | 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 (3)
| 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》 * |
| 王琛等: "《高分子材料改性技术》", 30 April 2007, 中国纺织出版社 * |
| 陈衍夏等: "《纤维材料改性》", 31 January 2009, 中国纺织出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102960913A (en) * | 2012-12-18 | 2013-03-13 | 金华冠华水晶有限公司 | Making process of artificial crystal diamond adhesive powder |
| 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 |
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| Publication number | Publication date |
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| CN102408867B (en) | 2013-08-21 |
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