CS244989B1 - Production method of shoe fusion cement - Google Patents
Production method of shoe fusion cement Download PDFInfo
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- CS244989B1 CS244989B1 CS849414A CS941484A CS244989B1 CS 244989 B1 CS244989 B1 CS 244989B1 CS 849414 A CS849414 A CS 849414A CS 941484 A CS941484 A CS 941484A CS 244989 B1 CS244989 B1 CS 244989B1
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- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000004568 cement Substances 0.000 title 1
- 230000004927 fusion Effects 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 14
- 229930195729 fatty acid Natural products 0.000 claims abstract description 14
- 239000000194 fatty acid Substances 0.000 claims abstract description 14
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 14
- 239000004831 Hot glue Substances 0.000 claims abstract description 8
- 239000000539 dimer Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000013638 trimer Substances 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 abstract description 11
- 230000001070 adhesive effect Effects 0.000 abstract description 11
- 239000002253 acid Substances 0.000 description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 5
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- -1 aliphatic diamine Chemical class 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002889 oleic acids Chemical class 0.000 description 1
- 150000002943 palmitic acids Chemical class 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polyamides (AREA)
Abstract
Vynález sa týká spůsobu výroby obuvnického tavného lepidla. Rieši problém sposobu polymerizácie dimérov mastných kyselin s cielom získania lepidla s krátkou otvorenou dobou. Podstata vynálezu spočívá v tom, že polymerizácia sa uskutečňuje v troch stupňoch, kde v prvom stupni teplota reakcie nie je vyššia ako teplota varu aminu s najnižšou číselnou hodnotou o viac ako 20 °C pri tlaku do 0,1 MPa po dobu 1 až 3 hodin v druhom stupni sa zvýši teplota reakcie na 160 až 170 °C pri tlaku do 0,25 MPa po dobu 3 až 5 hodin, v treťom stupni sa uskutoční doreagovanie pri teplote 200 až 220 °C pri tlaku do 0,5 MPa po dobu 1 až 5 hodin a potom sa odstráni reakčná voda.The present invention relates to a shoe making process hot melt adhesive. It solves the problem of cause polymerization of fatty acid dimers to obtain a short open adhesive time. The essence of the invention is that polymerization takes place in three stages, where at the first stage the reaction temperature is not higher than the lowest boiling point of the amine numerical value of more than 20 ° C under pressure up to 0.1 MPa for 1 to 3 hours in the second the reaction temperature is increased to 160 ° C up to 170 ° C at a pressure of up to 0.25 MPa for 3 up to 5 hours, in the third stage reacting at 200-220 ° C at room temperature pressure up to 0.5 MPa for 1 to 5 hours a then the reaction water is removed.
Description
Vynález sa týká sposobu výroby obuvnického tavného· lepidla polymerizáciou mastných kyselin, obsahujúcich 70 až 95 hmotn. dielov dimérov mastných kyselin, připadne až do 30 hmotn. dielov trimérov mastných kyselin na 100 hmotn. dielov zmesi mastných kyselin, za přítomnosti dikarboxylovej kyseliny s počtom atómov uhlíka 2 až 8 a monokarboxylových alifatických kyselin s ukončeným polymérnym refazcom s počtom atómov uhlíka 3 až 20.The present invention relates to a process for producing a shoe melt adhesive by fatty acid polymerization containing 70 to 95 wt. % of fatty acid dimers, up to 30 wt. parts of fatty acid trimers per 100 wt. parts of a mixture of fatty acids in the presence of a dicarboxylic acid having a carbon number of 2 to 8 and monocarboxylic aliphatic acids having a terminated polymeric chain having a carbon number of 3 to 20.
V obuvníckej výrobě pri zhotovovaní lemovaných napínacích stielok, pri napínaní stráň obuvi, pri zhotovovaní termotužiniek sa používajú tavné lepidlá, ktoré sú charakterizované ostrou teplotou topenia. Vlastnosti lepidiel sú ovplyvňované sposobom ich výroby. V súčasnosti je známy sposob výroby tavného· lepidla, ktoré pozostáva z dimérov mastných kyselin, s obsahom diméru 80 hmot. d. na 100 hmot. d. mastných kyselin, ďalej obsahuje dvojsýtne kyseliny a 1,2-diaminoetán. Reakcia sa uskutočňuje pri teplote 150 až 300 CC po dobu 5 hodin za následného oddestilovania vody. Známe je tiež tavné lepidlo připravené z dimérov mastných kyselin, dvojsýtnych kyselin, etyléndiamínu pri iniciačnej teplote nie vyššej ako 160 °C, minimálně 1 hodinu a nasledovnom dokondenzovaní pri teplote 175 až 2>25° Celsia za vzniku produktu, ktorý je rozpustný v butylalkohole. Známe je tavné lepidlo, ktoré obsahuje polyamidovú živicu, ktorá sa získala polykondenzáciou alifatického diamínu so zmesou nenasýtených monomérov a polymérov mastnej kyseliny a alifatické] dikarboxylovej kyseliny a/alebo esteru. Za výhodný sa považuje aj obsah prírodného alebo syntetického vosku. Ďalej je známe tavné lepidlo, ktoré sa připravuje polykondenzáciou diamínov s polymérnymi mastnými kyselinami alebo ich estermí, pričom obsah diméru kyseliny je 90 až 100 hmot. dielov. Polykondenzácia sa uskutočňuje pri teplote 180 až 250 °C. Nevýhodou uvedených lepidiel vyrobených uvedeným spůsobom je ich dlhšia doba tuhnutia a nižšia pevnosť spojov lepených materiálov.In the shoemaking industry, in the manufacture of lined stretch insoles, in the shoe sides, in the manufacture of thermo-binders, hot-melt adhesives are used, which are characterized by a sharp melting point. The properties of adhesives are influenced by the way they are produced. A process for the production of a hot melt adhesive consisting of fatty acid dimers having a dimer content of 80 wt. d. per 100 wt. d. fatty acids, further comprising dibasic acids and 1,2-diaminoethane. The reaction is carried out at 150 to 300 ° C for 5 hours, followed by distilling off the water. Also known is a hot melt adhesive prepared from dimers of fatty acids, dibasic acids, ethylenediamine at an initiation temperature of not more than 160 ° C for at least 1 hour and subsequent condensing at 175-225 ° C to give a product which is soluble in butyl alcohol. A hotmelt adhesive is known which comprises a polyamide resin obtained by polycondensation of an aliphatic diamine with a mixture of unsaturated monomers and polymers of fatty acid and aliphatic dicarboxylic acid and / or ester. The content of natural or synthetic wax is also preferred. Furthermore, a hot-melt adhesive is known which is prepared by polycondensation of diamines with polymeric fatty acids or their esters, wherein the acid dimer content is 90 to 100% by weight. parts. The polycondensation is carried out at a temperature of 180 to 250 ° C. The disadvantages of the adhesives produced by the above method are their longer setting time and lower bond strength of the glued materials.
Uvedené nevýhody odstraňuje sposob podlá vynálezu, ktorého· podstata spočívá v tom, že polymerizácia sa uskutočňuje v· troch stupňoch, kde v prvom stupni teplota reakcie nie je vyššia ako teplota varu aminu s nainižšou číselnou hodnotou o· viac ako 20 °C pri tlaku do 0,1 MPa po dobu 1 až 3 hodin, v druhom stupni sa zvýši teplota reakcie na 160 až 170 °C pri tlaku do 0,25 MPa po dobu 3 až 5 hodin, v treťom stupni sa uskutoční doreagovanie pri teplote 200 až 220 °C pri tlaku do· 0,5 MPa po dobu 3 až 5 hodin, potom sa odstráni reakčná voda.The above-mentioned disadvantages are overcome by the process according to the invention, which consists in that the polymerization is carried out in three stages, in which in the first stage the reaction temperature is not higher than the boiling point of the amine with the numerical value below 0.1 MPa for 1 to 3 hours, in the second step the reaction temperature is raised to 160 to 170 ° C under a pressure of up to 0.25 MPa for 3 to 5 hours, in the third step the reaction is carried out at 200 to 220 ° C at a pressure up to 0.5 MPa for 3-5 hours, then remove the water of reaction.
Technický účinok sposobu podlá vynálezu spočívá v tom, že sa připraví tavné lepidlo, ktoré má ikrátku otvorenú dobu, maximálně 10 sekúnd, počas ktorej sa dosiahne konečná pevnosť spoja zlepovaných materiálov. Týmto sa skráti doba lepenia.The technical effect of the process according to the invention is to provide a hot-melt adhesive which has an open time of at most 10 seconds, during which the final bond strength of the materials to be bonded is reached. This shortens the bonding time.
Sposob výroby lepidla ozrejmujú následovně příklady, kde množstva zložiek sú uvádzané z hmotnostných dieloch.The adhesive manufacturing process is illustrated by the following examples, wherein the amounts of the components are given in parts by weight.
Příklad 1Example 1
Do reakčnej nádoby sa nadávkovala zmes obsahujúci 190 hmotn. d. diméru kyseliny palmitovej a 10 hmotn. d. kyseliny palmitovej, 2 hmot. d. kyseliny adipovej, 26 hmot. d, etyléndiamínu a 3 hmot. diely kyseliny olejovej. Zmes sa polymerizovala v troch stupňoch. V prvom stupni sa zahriala na teplotu 110 °C pri tlaku do 0,1 MPa po dobu 2 hodin. V druhom stupni sa teplota zvýšila na 170 CC pri tlaku do 0,25 MPa po dobu 5 hodin. V treťom stupni sa zvýšila teplota na 200 °C pri tlaku do 0,5 MPa po dobu 4 hodin. Potom sa odstránila reakčná voda pomocou vákuovej vývevy. Takto připravené lepidlo· sa vypustilo a granulovalo. Lepidlo· bolo křehké s nasledovnými fyzikálno-mechanickými vlastnosťami:A mixture containing 190 wt. d. % palmitic acid dimer and 10 wt. d. palmitic acid, 2 wt. d. adipic acid, 26 wt. d, ethylenediamine and 3 wt. parts of oleic acid. The mixture was polymerized in three stages. In the first stage, it was heated to 110 ° C at a pressure of up to 1 bar for 2 hours. In the second step, the temperature was raised to 170 ° C at a pressure of up to 50 psi for 5 hours. In the third step, the temperature was raised to 200 ° C at a pressure of up to 0.5 MPa for 4 hours. The reaction water was then removed by means of a vacuum pump. The adhesive thus prepared was discharged and granulated. The adhesive · was brittle with the following physico-mechanical properties:
teplota maknutia číslo kyslosti aminové číslo viskozita pri 165 °Cmilling temperature acid number amine number viscosity at 165 ° C
110 °C max. 10 max. 7 2 500 mPa . s110 ° C max. 10 max. 7 2,500 mPa. with
Příklad 2Example 2
Do reakčnej nádoby sa nadávkovala zmes obsahujúca 160 hmot. d. diméru kyseliny olejovej, 30 hmot. d. triméru kyseliny olejovej a 10 hmot. d. kyseliny olejovej, 10 hmot. d. kyseliny aselaikovej, 28 hmot. dielov etyléndiamínu a 4 hmot. d. kyseliny palmitovej. Zmes sa polymerizovala v troch stupňoch. V prvom stupni sa zahriala na teplotu 120 °C pri tlaku do 0,1 MPa po· dobu 1 hodiny. V druhom stupni sa teplota zvýšila na 160 °C pri tlaku do 0,25 MPa po dobu 5 hodin. V treťom stupni sa zvýšila teplota na 220 °C pri tlaku do 0,5 MPa po dobu 3 hodin. Potom sa odstránila reakčná voda pomocou vákuovej vývevy. Takto připravené lepidlo sa vypustilo a granulovalo. Lepidlo bolo· křehké s nasledovnými fyzikálno-mechanickými vlastnosťami:A mixture containing 160 wt. d. oleic acid dimer, 30 wt. d. oleic acid trimer and 10 wt. d. oleic acid, 10 wt. d. aselaic acid, 28 wt. parts of ethylenediamine and 4 wt. d. palmitic acid. The mixture was polymerized in three stages. In the first step, it was heated to 120 ° C at a pressure of up to 1 bar for 1 hour. In the second stage, the temperature was raised to 160 ° C at a pressure of up to 50 psi for 5 hours. In the third stage, the temperature was raised to 220 ° C under a pressure of up to 0.5 MPa for 3 hours. The reaction water was then removed by means of a vacuum pump. The adhesive thus prepared was drained and granulated. The adhesive was brittle with the following physico-mechanical properties:
teplota maknutia číslo kyslosti aminové číslo viskozita pri 210 °Cmilling temperature acid number amine number viscosity at 210 ° C
170 CC max. 10 max. 7 3 000 mPa . 3170 C C max. 10 max. 7 3000 mPa. 3
Příklad 3Example 3
Do reakčnej nádoby sa nadávkovala zmes obsahujúca 160 hmot. d. kyseliny stearovej a 40 hmot. d. triméru kyseliny stearovej, 23 hmot. d. kyseliny sebakovej, 26 hmot. d. etyléndiamínu, 13 hmot. d. hexametyléndiamínu a 8 hmot. d. kyseliny stearovej. Zmes sa polymerizovala v troch stupňoch. V prvom stupni sa zahriala na teplotu 115 °C pri tlaku do 0,1 MPa po dobu 1,5 hodiny.A mixture containing 160 wt. d. stearic acid and 40 wt. d. stearic acid trimer, 23 wt. d. sebacic acid, 26 wt. d. ethylenediamine, 13 wt. d. hexamethylenediamine and 8 wt. d. stearic acid. The mixture was polymerized in three stages. In the first stage, it was heated to 115 ° C at a pressure of up to 1 bar for 1.5 hours.
V druhom stupni sa teplota zvýšila na 165 °C pri tlaku do 0,25 MPa po dobu 4 hodin. V treťom stupni sa teplota zvýšila na 210 “C pri tlaku do 0,5 MPa po dobu 3,5 hodin. Potom sa odstránila reakčná voda použitím vákuovej vývěvy. Takto připravené lepidlo sa vypustilo a granulovalo. Lepidlo bolo elastické s nasledovnými fyzikálno-mecha nickými vlastnosťami:In the second stage, the temperature was raised to 165 ° C at a pressure of up to 0.25 MPa for 4 hours. In the third stage, the temperature was raised to 210 ° C at a pressure of up to 0.5 MPa for 3.5 hours. The reaction water was then removed using a vacuum pump. The adhesive thus prepared was drained and granulated. The adhesive was elastic with the following physico-mechanical properties:
teplota máknutia číslo kyslosti aminové Číslo viskozita pri 200 °Csoftening point acid number amine Viscosity number at 200 ° C
170 °C max. 10 max. 7 2 500 mPa . s170 ° C max. 10 max. 7 2,500 mPa. with
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS849414A CS244989B1 (en) | 1984-12-06 | 1984-12-06 | Production method of shoe fusion cement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS849414A CS244989B1 (en) | 1984-12-06 | 1984-12-06 | Production method of shoe fusion cement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS941484A1 CS941484A1 (en) | 1985-11-13 |
| CS244989B1 true CS244989B1 (en) | 1986-08-14 |
Family
ID=5444523
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS849414A CS244989B1 (en) | 1984-12-06 | 1984-12-06 | Production method of shoe fusion cement |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS244989B1 (en) |
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1984
- 1984-12-06 CS CS849414A patent/CS244989B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS941484A1 (en) | 1985-11-13 |
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