CS206068B1 - Method of making the high-reactive ureaformaldehyde bitumens - Google Patents

Method of making the high-reactive ureaformaldehyde bitumens Download PDF

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CS206068B1
CS206068B1 CS495579A CS495579A CS206068B1 CS 206068 B1 CS206068 B1 CS 206068B1 CS 495579 A CS495579 A CS 495579A CS 495579 A CS495579 A CS 495579A CS 206068 B1 CS206068 B1 CS 206068B1
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Czechoslovakia
Prior art keywords
urea
formaldehyde
reactive
weight
pressure
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CS495579A
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Czech (cs)
Slovak (sk)
Inventor
Michal Kellner
Frantisek Ambroz
Miroslav Host
Radislav Lipka
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Michal Kellner
Frantisek Ambroz
Miroslav Host
Radislav Lipka
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Application filed by Michal Kellner, Frantisek Ambroz, Miroslav Host, Radislav Lipka filed Critical Michal Kellner
Priority to CS495579A priority Critical patent/CS206068B1/en
Publication of CS206068B1 publication Critical patent/CS206068B1/en

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  • Phenolic Resins Or Amino Resins (AREA)

Description

(54) Sposob výroby vysokoreaktívnych močovinoformaldehydových živíc(54) Method of producing high-reactive urea-formaldehyde resins

Vynález rieši spósob výroby vysokoreaktívnych močovinoformaldehydových živíc vhodných ako poloprodukt pre přípravu celej rady modifikovaných lepidiel a ako vysokoreaktívne lepidlo pre dřevařsky priemysel a nábytkářský priemysel.The invention provides a process for the production of highly reactive urea-formaldehyde resins suitable as a semi-product for the preparation of a variety of modified adhesives and as a highly reactive adhesive for the wood and furniture industries.

PodTa doterajších diskontinuálnych postupov (NSR pat. 2,207 921 a 2 234 857) pri výrobě močovinoformaldehydových lepidiel sa reaktivita dosahuje změnou dávkovania surovin a úpravou reakčnej doby. Pracuje sa spravidla za normálneho tlaku a teplót do 100 °C. Spravidla obsah formaldehydu sa pohybuje v rozmedzí 1 ai 3 % hmotnostných a ako vysokoreaktívny typ živice nie sú vhodné.According to prior discontinuous processes (German Pat. Nos. 2,207,921 and 2,234,857) in the production of urea-formaldehyde adhesives, reactivity is achieved by varying the feed rate and adjusting the reaction time. As a rule, work is carried out at normal pressure and temperatures up to 100 ° C. As a rule, the formaldehyde content is between 1 and 3% by weight and is not suitable as a highly reactive type of resin.

V patentovej literatuře sa vyskytuje celý rad patentov zaoberajúcich sa přípravou močovinoformaldehydových živíc vhodných ako lepidla (Jap. pat. 74-18925 a 74.18928, NSR pat. 2 154 570, pCr pat. 74 080 a SalŠie), avšak výsledný produkt je celkom odlišný od produktu vyrobeného podlá tohto vynálezu. Obsah volného formaldehydu je v rozmedzí 1 až 3 % hmotných a reaktivita s chloridom amonným (15^-ný vodný roztok, 1 % na hmotu lepidla) pri 100 °C je vyššia ako 60 3ekúnd.There are a number of patents dealing with the preparation of urea-formaldehyde resins suitable as adhesives in the patent literature (Jap. Pat. 74-18925 and 74.18928, Germany Pat. the product produced according to the invention. The free formaldehyde content is in the range of 1 to 3% by weight and the reactivity with ammonium chloride (15% aqueous solution, 1% by weight of the adhesive) at 100 ° C is higher than 60 3 seconds.

Podstatou tohto vynálezu je spósob kontinuálnej výroby močovinoformaldehydových živíc v dvoch cirkulačnýoh reakčných okruhoch pri teplote 100 až 150 °C a tlakuThe present invention is based on a process for the continuous production of urea-formaldehyde resins in two circulating reaction circuits at a temperature of 100 to 150 ° C and pressure

206 068206 068

206 068206 068

0,002 až 0,5 MPa v prvom ciřkulačnom reakčnom okruhu, kde prebieha kondenzáoia v prí” tomnosti 0,01 až 0,5 % hmotnostných organiokýoh alebo anorganických kyselin, pričom základný molárny poměr vstupných surovin» močoviny a formaldehydu je 1:1,5 až 1:2,9 s výhodou 1:2,1. Močovinoformaldehyďový predkondenzát sa připravuje predom v samostatnou: miešanom aparáte a po úpravě pH s organickou alebo anorganickou kyselinou sa nastrekuje Serpadlom do tlakového reaktora.0.002 to 0.5 MPa in the first clarifying reaction circuit, where the condensation is carried out in the presence of 0.01 to 0.5% by weight of organo-organic or inorganic acids, the basic molar ratio of urea to formaldehyde starting materials being 1: 1.5 to 1: 2.9, preferably 1: 2.1. The urea-formaldehyde precondensate is prepared beforehand in a separate agitator and after adjusting the pH with an organic or inorganic acid, it is injected by Serpadl into a pressure reactor.

Produkt z prvého reakčného okruhu sa kontinuálně prepúsťa do druhého reakčného stupňa, kde pri tlaku 2,6 až 19,75 kPa je živica zahuštěná na obsah sušiny 50 až 70 % hmotnostných a viskozitu 500 až 2500 mPa.s, Obsah volného formaldehydu je 3 až 8 % hmotnostných, pH produktu sa upravuje prídavkom 0,01-0,5 % hydroxidu sodného na hodnoty 7 až 8,5.The product from the first reaction circuit is continuously transferred to the second reaction stage, where at a pressure of 2.6 to 19.75 kPa the resin is concentrated to a dry matter content of 50 to 70% by weight and a viscosity of 500 to 2500 mPa.s. The pH of the product is adjusted to pH 7-8.5 by addition of 0.01-0.5% sodium hydroxide.

**

Hotové lepidlo o obsahu volného formaldehydu 5 % je velmi reaktivně (želatinaoný Čas pri 100 °0 s chloridom amonným je 20 sekúnd) a poušiva sa v nabytkárskom a drevárskom priemysle napr. pre výrobu drevotrieskových dosák systémom Bartrew, připadne ako poloprodukt pre výrobu montážnych lepidiel a lepidiel pre rýchlodýhovanie.The ready-to-use 5% free formaldehyde adhesive is very reactive (gelatinous time at 100 ° 0 with ammonium chloride is 20 seconds) and is used in the furniture and woodworking industry e.g. for the production of particle board with the Bartrew system, eventually as a semi-product for the production of assembly adhesives and adhesives for rapid veneering.

PřikladExample

Do aparátu s možnosťou ohladenia a miešania sa nadávkuje 19 600 1 formalínu o koncentráoií 37 % hmotnostných, přidá 12 1 10%-ného hydroxidu sodného na úpravu pH v rozmedzí 7 až 8,5 a přidá sa 8 200 kg pevnej močoviny. Po jej rozpuštění sa přidá lOJž-ná kyselina mravenoia v takom množstve, aby pH bolo v rozmedzí 5 až 7»9. Takto pri pravený predkondenzát (molárny poměr močoviny a formaldehydu 1:1,95) sa dávkuje do prvého reakčného stupňa, kde pri teplote 120 °0 a tlaku 0,25 MPa prebieha kondenzaoná reakcia. Produkt z prvého reakčného stupna o viskozite 20 až 80 mPa.s sa odoberá do druhého reakčného stupňa, kde sa zahustí na obsah sušiny 66 aŽ 1% a vizkoZitu 1200 mPa e, pri teplote 55 °C a tlaku 10,0 kPa. Do druhého stupňa sa zároveň kontinuálně přidává 10%-ný hydroxid sodný tak, aby výsledné pH bolo 7»5»19,600 L of 37% by weight of formalin, 12 L of 10% sodium hydroxide to adjust the pH in the range of 7-8.5, and 8,200 kg of solid urea are added to the smoothing and mixing apparatus. After dissolution, 10% formic acid is added in an amount such that the pH is in the range 5-7-9. Thus prepared precondensate (molar ratio of urea to formaldehyde of 1: 1.95) is fed to the first reaction stage, where a condensation reaction takes place at a temperature of 120 ° C and a pressure of 0.25 MPa. The product of the first reaction stage having a viscosity of 20 to 80 mPa.s is taken to the second reaction stage, where it is concentrated to a dry matter content of 66-1% and a viscosity of 1200 mPa.s at 55 ° C and 10.0 kPa. 10% sodium hydroxide is continuously added to the second stage so that the resulting pH is 7 »5»

Claims (2)

PREDMET VYNÁLEZUOBJECT OF THE INVENTION 1. SpSsob výroby vysokoreaktívnyoh mooovinófófmaldehydovýoh živio pre použitie v drevárskom a nábytkářském priemysle vyznačujúoi sa týjfi, že predkondenzát močoviny a formaldehydu kondenzuje v dvojstupňovom kontinuálnem usporiadaní pri tlaku v 1. stupni 0,002 aŽ 0,5 MPa, teplóté 100-150 °Ó a molárnom pomere močoviny a formaldehydu 1:1,5 až 1:2,9 s výhodou 1:2,1 za přítomnosti 0,01 až 0,5 % hmotnostných organických, alebo anorganických kyselin, v druhom stupni sa zahustí1. A process for the production of high-reactive mono-amino-phthaldehyde nutrient for use in the wood and furniture industry, characterized in that the urea-formaldehyde precondensate is condensed in a two-stage continuous arrangement at a pressure of 1 to 100 bar, at a temperature of 100-150 °. urea and formaldehyde 1: 1.5 to 1: 2.9, preferably 1: 2.1, in the presence of 0.01 to 0.5% by weight of organic or inorganic acids; 206 066 pri tlaku 2,60 až 19,75 kPa na obsah sušiny 50 až 70 % hmotnostných a zalkalizuje prídavkom hjřdroxidu sodného v množstve 0,01 až 0,5 % na pH 7 až 8,5.206 066 at a pressure of 2.60 to 19.75 mbar to a dry matter content of 50 to 70% by weight, and made basic by addition of sodium hj ° droxidu 0.01 to 0.5% at a pH of 7 to 8.5. 2, SpSsob podl’a bodu 1, vyznačujúci sa tým, še sa použije predkondenzát predom připravený v samostatnom miešanom aparáte rozpuštěním pevnej močoviny vo vodnom roztoku formaldehydu.2. The method of claim 1, wherein the precondensate previously prepared in a separate agitator is used by dissolving the solid urea in an aqueous formaldehyde solution.
CS495579A 1979-07-16 1979-07-16 Method of making the high-reactive ureaformaldehyde bitumens CS206068B1 (en)

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