CS257363B1 - Production method of ureaformaldehyde condensate with special features - Google Patents
Production method of ureaformaldehyde condensate with special features Download PDFInfo
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- CS257363B1 CS257363B1 CS866971A CS697186A CS257363B1 CS 257363 B1 CS257363 B1 CS 257363B1 CS 866971 A CS866971 A CS 866971A CS 697186 A CS697186 A CS 697186A CS 257363 B1 CS257363 B1 CS 257363B1
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- Czechoslovakia
- Prior art keywords
- urea
- formaldehyde
- addition
- molar ratio
- pressure
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- 229920001807 Urea-formaldehyde Polymers 0.000 title claims abstract description 9
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 39
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract 2
- 239000011575 calcium Substances 0.000 claims abstract 2
- -1 calcium organic acid salts Chemical class 0.000 claims abstract 2
- 229910021538 borax Inorganic materials 0.000 claims description 5
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 5
- 239000004328 sodium tetraborate Substances 0.000 claims description 5
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 159000000000 sodium salts Chemical class 0.000 claims description 4
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 239000004281 calcium formate Substances 0.000 claims description 3
- 229940044172 calcium formate Drugs 0.000 claims description 3
- 235000019255 calcium formate Nutrition 0.000 claims description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- 238000006068 polycondensation reaction Methods 0.000 claims description 2
- 239000003292 glue Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000009257 reactivity Effects 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000004848 polyfunctional curative Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 240000000731 Fagus sylvatica Species 0.000 description 1
- 235000010099 Fagus sylvatica Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Rieši sa spůsob výroby močovinoformaldehydových kondenzátov so specifickými vlastnosťami vhodný ako lepidlo v drevárskom a nábytkárskom priemysle, ktoré sa připravuje adíciou močoviny a formaldehydu v mólovom pomere U : F 1 : 1,6 až 1: 2,2 pri pH 3,5 až 8 s výhodou 6,5 tento predkondenzát sa ďalej kontinuálně spracováva pri teplote 102 až 150 °C, tlaku 0,002 až 0,5 MPa a v druhom stupni sa dalej kondenzuje za vákua, pri teplote 40 až 80 °C za kontinuálneho přídavku vodného roztoku močoviny s prídavkom 0,01 až 5 % vápenatej soli organickej kyseliny. Množstvo močoviny do druhého stupňa odpovedá úpravě koncového mólového poměru U : F 1:1,5 až 1:1,86.The process for the production of urea-formaldehyde is solved condensates with specific properties suitable as glue in woodworking and the furniture industry by the addition of urea and formaldehyde in the U: F molar ratio of 1: 1.6 to 1: 2.2 at pH 3.5 to 8, preferably 6.5 this precondensate is further processed continuously at a temperature of 102 to 150 ° C, a pressure of 0.002 to 0.5 MPa and in the second stage is further condensed under vacuum at 40-80 ° C with continuous stirring by adding an aqueous urea solution with the addition of 0.01 to 5% calcium organic acid salts. Amount of urea the second level corresponds to the adjustment end molar ratio U: F 1: 1.5 to 1: 1.86.
Description
Vynález rieši sposob výroby močovinoformaldehydových kondenzátov so specifickými vlastnosťami obsahujúce aditivum, určenými ako lepidlo v drevárskom a nábytkárskom priemysle pri dýhování a ako montážně lepidlo, ktoré má dobré lepiace vlastnosti za studená za súčasnej jeho zníženej reaktivity po přidaní tužidla, pričom vplyvom aditíva dochádza zároveň k zvýšeniu pevnosti.The invention provides a process for the production of urea-formaldehyde condensates with specific additive-containing properties intended as an adhesive in the wood and furniture industry in veneering and as an assembly adhesive having good cold adhesive properties while reducing its reactivity after hardener addition. strength.
Podfa doterajšícb postupov chráněných AO 209 101 sa vyrábajú močovinoformaldehydové kondenzáty vhodné ako lepidla v drevárskom a nábytkárskom priemysle z vodného roztoku močoviny a formaldehydu dvojstupňovou polykondenzáciou, kde v prvom stupni pri teplote 102 až 150 °C, tlaku 0,002 až 0,5 MPa v prietočnom kontinuálnom zariadení so základným molovým pomerom vstupných surovin močoviny s formaldehydu 1 : 1,5 až 1 : 2,2 s výhodou 1 : : 1,95 za přítomnosti 0,001 až 0,495 % hmot., s výhodou 0,005 % hmot. organickej, alebo anorganickej kyseliny s výhodou kyseliny mravčej prebehne kondenzácia. V druhom stupni sa ďalej kondenzuje pri tlaku 2 až 20 kPa, pri teplote 30 až 90 °C za kontinuálneho přídavku vodného roztoku močoviny o koncentrácii 20 až 80 % hmot., s výhodou 50% hmot. a to v takom množstve, aby výsledný mólový poměr močoviny s formaldehydu bol 1 : 1,3 až 1 : 1,85 a kontinuálneho dávkovania roztoku hydroxidov alkalických kovov, alebo alkalických zemin.Prior art processes protected by AO 209 101 produce urea-formaldehyde condensates suitable as adhesives in the wood and furniture industry from aqueous urea-formaldehyde solution by two-stage polycondensation, where in a first stage at a temperature of 102 to 150 ° C, a pressure of 0.002 to 0.5 MPa in a continuous flow devices having a basic molar ratio of feedstocks of urea with formaldehyde of 1: 1.5 to 1: 2.2, preferably 1: 1.95 in the presence of 0.001 to 0.495% by weight, preferably 0.005% by weight. organic or inorganic acid, preferably formic acid, is condensed. In the second step, it is further condensed at a pressure of 2 to 20 kPa, at a temperature of 30 to 90 ° C with the continuous addition of an aqueous urea solution having a concentration of 20 to 80% by weight, preferably 50% by weight. in such an amount that the resulting molar ratio of urea to formaldehyde is 1: 1.3 to 1: 1.85 and the continuous dosing of the alkali metal or alkaline earth hydroxide solution.
Ďalšie postupy přípravy podobných typov UF kondenzátov (NSR patent 2 287 921, 2 444 856) chránia postupy přípravy vo velmi kyslom prostředí (pH výrazné pod hodnotu 5), připadne NSR pat. 2109 754 pracuje kontinuálně v miešaných kaskádových reaktorech za přítomnosti aminokyselin pri meniacom sa pH od 4,2 až 8,0 za normálného tlaku.Other processes for the preparation of similar types of UF condensates (U.S. Pat. No. 2,287,921, 2,444,856) protect the processes of preparation in a very acidic environment (pH significantly below 5), or the NSR Pat. 2109,754 operates continuously in stirred cascade reactors in the presence of amino acids at varying pH from 4.2 to 8.0 at normal pressure.
Z ekonomických dovodov, pokial výrobea UF kondenzátov je zároveň výrobcom formaldehydu, sa vytvárajú UF kondenzáty s formaldehydu o nízkom obsahu stabilizačného metanolu podfa AO 226 922 (výrazná úspora metanolu), tým sa však dosahuje vysoká reaktivita UF kondenzátorov.From economic reasons, when the production of UF condensates is also a formaldehyde producer, UF condensates are formed with formaldehyde having a low stabilizing methanol content according to AO 226 922 (significant methanol savings), but this results in a high reactivity of the UF capacitors.
Pre praktické použitie je však důležité, aby výsledná živica, ktorá sa používá ako pojidlo v drevárskom a nábytkárskom priemysle málo schopnost změny — regulácie reaktivity (hlavně zníženle) po přídavku tužidla. Tento požiadavok vznikol rozšířením sortimentu lepidlel pre maloodberatefov v celej ČSSR.For practical use, however, it is important that the resulting resin, which is used as a binder in the wood and furniture industry, has little ability to change - reactivity regulation (mainly reduced) after hardener addition. This requirement was created by extending the range of adhesives for small customers throughout the CSSR.
Podstatou tohoto vynálezu je spósob kontinuálnej výroby močovinoformaldehydových živíc pri teplote 102 až 150 °C a tlaku 0,002 až 0,5 MPa v prietočnom kontinuálnom zariadení, pričom základný mólový poměr vstupných surovin močoviny a formaldehydu je 1 :1,6 až 1 : 2,2 s výhodou 1:1,95. Močovinoformaldehydový predkondenzát sa připravuje predom v ©amostatnom aparáte s formaldehydu, ktorého pH bolo upravené prídavkom hydroxidu alkalického kovu, hydroxidu alkalických zemin, alebo sodnou sofou kyseliny boritej, alebo jej derivátov s výhodou tetraboritanom sodným na hodnoty pH 3,5 až 8,0 s výhodouSUMMARY OF THE INVENTION The present invention provides a process for the continuous production of urea-formaldehyde resins at a temperature of 102 to 150 ° C and a pressure of 0.002 to 0.5 MPa in a continuous flow device, wherein the basic mole ratio of urea to formaldehyde feedstocks is 1: 1.6 to 1: 2.2 preferably 1: 1.95. The urea-formaldehyde precondensate is prepared beforehand in a separate formaldehyde apparatus, the pH of which has been adjusted by the addition of an alkali metal hydroxide, an alkaline earth hydroxide, or a sodium salt of boric acid or its derivatives, preferably sodium tetraborate, to pH 3.5 to 8.0.
4.5 a pevnej močoviny. Tento predkondenzát sa dávkuje do tlakového reaktora, kde prebieha prvý stupeň kondenzácie.4.5 and solid urea. This precondensate is fed to a pressure reactor where the first condensation stage takes place.
V druhom reakčnom stupni prebieha ďalšia kondenzácia přidávaného vodného roztoku močoviny, ktorý obsahuje 0,01 až 5 % vápenatej soli organickej kyseliny s výhodou mravčanu vápenatého. Vlastná kondenzácia prebieha pri tlaku 2 až 20 kPa a teplote 30 až 80 °C, pH 7 až 9 s výhodou 8,2. Komponenty sú do druhého stupňa dávkované kontinuálně, pričom pH sa upravuje prídavkom hydroxidov alkalických kovov, alebo alkalických zemin, alebo sodnou sofou kyseliny boritej, alebo jej derivátov s výhodou tetraboritanom sodným. Celkové dávkované množstvo močoviny je také, aby výsledný mólový poměr močoviny a formaldehydu bol 1 : 5 až 1 : 1,85.In the second reaction step, further condensation of the added aqueous urea solution is carried out, which contains 0.01 to 5% calcium salt of an organic acid, preferably calcium formate. The actual condensation takes place at a pressure of 2 to 20 kPa and a temperature of 30 to 80 ° C, a pH of 7 to 9, preferably 8.2. The components are metered to the second stage continuously, the pH being adjusted by the addition of alkali metal or alkaline earth hydroxides, or a sodium salt of boric acid or derivatives thereof, preferably sodium tetraborate. The total amount of urea dosed is such that the resulting molar ratio of urea to formaldehyde is 1: 5 to 1: 1.85.
Podfa tohoto vynálezu sa získá jednoduchou technológiou živica s viskozitou 400 až 1 800 mPa. s, ktorá je vhodná ako lepidlo pre drevársky a nábytkářský priemysel, ktorá podfa obsahu retardujúcej zložky—vápenatej soli organickej kyseliny má schopnost změny reaktivity po přidaní tužidla napr.: chloridu amonného.According to the invention, a resin with a viscosity of 400 to 1800 mPa is obtained by simple technology. s, which is suitable as an adhesive for the wood and furniture industry, which, according to the content of the retardant component - calcium salt of the organic acid, has the ability to change the reactivity after addition of a hardener, for example: ammonium chloride.
Lepidlo podfa příkladu 1 je možné použit’ ako montovne lepidlo (za studená], alebo ako dýhovacie lepidlo v nábytkárskom priemysle.The adhesive of Example 1 can be used as a fitting adhesive (cold) or as a veneer adhesive in the furniture industry.
Příklad 1Example 1
Do zásobníka opatřeného miešadlom s možnosťou chladenia sa nadávkuje 15 m3 vodného roztoku formaldehydu o koncentrácii 37,1 % hmotnostných, přidá sa 20 1 10 %-ného vodného roztoku tetraboritanu sodného na úpravu pH, ktoré je po úpravě v rozmedzi 3,5 až 7 a přidá sa 12 500 kg pevnej močoviny. Po jej rozpuštění predkondenzát močoviny a formaldehydu (mólový poměr 1 : 1,95) sa dávkuje v množstve 8 až 12 m3/h do prvého reakčného stupňa, kde pri teplote 125 °C a tlaku 0,3 MPa prebieha kondenzačně reakcia. Produkt z prvého stupňa o viskozite 35 až 100 mPa. s sa kontinuálně odoberá do druhého reakčného stupňa, kde prebieha druhý stupeň kondenzácie prídavkom 1,3 až 1,6 m3/h 50 %-ného roztoku močoviny s obsahomA 15 m 3 aqueous solution of formaldehyde at a concentration of 37.1% by weight is added to a container equipped with a stirrer with cooling and 20 l of a 10% aqueous solution of sodium tetraborate is added to adjust the pH, which is between 3.5 and 7 after adjustment. and add 12,500 kg of solid urea. After dissolution of the urea-formaldehyde precondensate (molar ratio 1: 1.95), 8 to 12 m 3 / h are metered into the first reaction stage, where a condensation reaction takes place at 125 ° C and 0.3 MPa. First-stage product having a viscosity of 35 to 100 mPa. s is taken continuously to the second reaction stage, where the second stage of condensation takes place by the addition of 1.3 to 1.6 m 3 / h of a 50% urea solution containing
1.5 % hm. mravčanu vápenatého a kontinuálneho přídavku 10 %-ného vodného roztoku tetraboritanu sodného tak, aby pH bolo v rozmedzi 7,0 až 9,0, pri teplote 60 °C a tlaku 10,2 kPa,1.5% wt. calcium formate and the continuous addition of a 10% aqueous solution of sodium tetraborate such that the pH is between 7.0 and 9.0, at a temperature of 60 ° C and a pressure of 10.2 kPa,
Produkt z druhého reakčného stupňa sa kontinuálně odoberá, ochladzuje. Obsahuje cca 67 % hmot. UF živice, jeho viskozita jeThe product from the second reaction step is continuously removed, cooled. It contains approx. UF resin, its viscosity is
900 mPa. s, obsah volného formaldehydu900 mPa. s, free formaldehyde content
2,5 % hmot., reaktivita 100 min/20 °C s chloridem amonným ako tužidlom. Pevnost' lepeného spoja na bukovéj preglejke po teste IF—20 je 2,1 MPa.2.5 wt%, reactivity 100 min / 20 ° C with ammonium chloride as a hardener. The bond strength on the beech plywood after the IF-20 test is 2.1 MPa.
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Application Number | Priority Date | Filing Date | Title |
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CS866971A CS257363B1 (en) | 1986-09-29 | 1986-09-29 | Production method of ureaformaldehyde condensate with special features |
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CS866971A CS257363B1 (en) | 1986-09-29 | 1986-09-29 | Production method of ureaformaldehyde condensate with special features |
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Publication Number | Publication Date |
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CS697186A1 CS697186A1 (en) | 1987-09-17 |
CS257363B1 true CS257363B1 (en) | 1988-04-15 |
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CS866971A CS257363B1 (en) | 1986-09-29 | 1986-09-29 | Production method of ureaformaldehyde condensate with special features |
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CS (1) | CS257363B1 (en) |
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1986
- 1986-09-29 CS CS866971A patent/CS257363B1/en unknown
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CS697186A1 (en) | 1987-09-17 |
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