CS201871B1 - Process for preparing crosslinked foamed polypropylene - Google Patents

Process for preparing crosslinked foamed polypropylene Download PDF

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CS201871B1
CS201871B1 CS793278A CS793278A CS201871B1 CS 201871 B1 CS201871 B1 CS 201871B1 CS 793278 A CS793278 A CS 793278A CS 793278 A CS793278 A CS 793278A CS 201871 B1 CS201871 B1 CS 201871B1
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polypropylene
product
foamed polypropylene
crosslinked foamed
weight
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CS793278A
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Czech (cs)
Slovak (sk)
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Vojtech Palenik
Andrej Romanov
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Vojtech Palenik
Andrej Romanov
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Description

Vynález rieši spósob přípravy zosieteného Tahčeného polypropylénu.SUMMARY OF THE INVENTION The present invention provides a process for preparing crosslinked drawn polypropylene.

Celý rad patentov sa týká obecne Tahčenia polyolefínov, připadne ich zmesi a Tahčenie polypropylénu je v nich uvedené iba ako jeden z príkladov. V dósledku toho literatúra, ktorá sa zaoberá přípravou Tahčeného polypropylénu, zohladňujúce jeho Specifické, fyzikálně a chemické vlastnosti, je relativné nepočetná. Relativné málo je přepracovaná problematika Tahčenia polypropylénu za súčasného zosietenia polymérovej matrice organickými peroxidmi.A number of patents generally relate to the drawing of polyolefins, or mixtures thereof, and the drawing of polypropylene is given only as one example. As a result, the literature dealing with the preparation of Drawn polypropylene, taking into account its specific, physical and chemical properties, is relatively small. The issue of drawing polypropylene while crosslinking the polymer matrix with organic peroxides is relatively low.

Postupy na přípravu Tahčeného polypropylénu možno rozdeliť podTa toho, čí k 1’ahčeniu dochádza bez zosietenia polyméru alebo sa polypropylén v procese Tahčenia zosieti. Príkladom Tahčenia polypropylénu bez jeho zosietenia je patent (Jap. patent 75 28 110), podlá ktorého sa získá 1’ahčený produkt polypropylénu, azobisformamidu, stearátu zinočnatého a kvapalného parafínu za použitia dvoch vytláčacích strojov.The processes for preparing the drawn polypropylene can be divided according to whether the drawing takes place without crosslinking the polymer or the polypropylene crosslinks in the drawing process. An example of a drawing of polypropylene without crosslinking thereof is a patent (Japanese Patent 75 28 110) which provides a lightweight polypropylene product, azobisformamide, zinc stearate and liquid paraffin using two extruders.

Lahčený polypropylén so zosietenou polymérovou matricou bol připravený zo zmesi polypropylénu, trialylkyanurátu a azobisformamidu, pričom sa zmes ožiarila prúdom elektronov za účelom zosietenia polyméru (Jap. pat. vykl. spis 75 09 668).Bottled polypropylene with a crosslinked polymer matrix was prepared from a blend of polypropylene, trialyl cyanurate and azobisformamide, irradiating the mixture with an electron beam to crosslink the polymer (Japanese Pat. No. 75 09 668).

Peroxidy sa použili na zosietenie polypropylénu pri príprave Tahčeného produktu spolu s divinylbenzénom a azobisformamidom ako nadúvadlom (Jap. pat. 70 41 098).Peroxides were used to cross-link polypropylene in the preparation of the drawn product together with divinylbenzene and azobisformamide as blowing agent (Jap. Pat. 70 41 098).

Doteraz známe postupy na přípravu zosieteného Tahčeného polypropylénu využívajú teda viacfunkčné monoméry (napr. divinylbenzén, trialylkyanurát) v kombinácii bu3 s organickýmHitherto known processes for the preparation of crosslinked drawn polypropylene utilize multifunctional monomers (e.g., divinylbenzene, trialyl cyanurate) in combination with either organic and organic.

201 871 peroxidom alebo vhodným žiarením a nadúvadlo (napr. azobieformamid), ktoré pri podmienkach 1’ahčenia poskytuje plyny na vytváranie penovej átruktúry.201 871 with peroxide or suitable radiation and a blowing agent (eg azobieformamide) which, under the conditions of l'auging, provides gases for forming a foam structure.

Podstata vynálezu spočívá v tom, Se sa k práškovému polypropylénu pri izbovej teplote primieša t-butylperbenzoát v koncentrácii 3 až 12 % hmotnostných a nenasýtená zlúčenina obecného vzorca:The principle of the invention consists in admixing t-butyl perbenzoate in a concentration of 3 to 12% by weight to the polypropylene powder at room temperature and an unsaturated compound of the formula:

X ch2 = é - C - O - (R-,) l'nX ch 2 = é - C - O - (R 1 -) 1'n

O - (C - R- - C - 0)O - (C - R - - C - 0)

N 2 ll m O 0N 2 m m 0

X (Bl>n - 0 - C - C = CH2 kde X je H alebo CH-j, je zbytok glykolu, R2 je zbytok alifatickej alebo aromatickej dikarbbxylovej kyseliny, n mdže nadobudnúť hodnoty 1 až 3, m = O alebo 1, v koncentrácii 0,5 až 10 % hmotnostných, zmes sa pri zvýáenom tlaku vyhřeje na teplotu 443 až 458 K a po uvolnění tlaku vznikne l’ahčený produkt.X (B1> n -O-C-C = CH 2 where X is H or CH-j, is a glycol residue, R 2 is an aliphatic or aromatic dicarbonyl acid residue, n may have values of 1 to 3, m = 0 or 1 at a concentration of 0.5 to 10% by weight, the mixture is heated to a temperature of 443 to 458 K at elevated pressure, and a light product is formed when pressure is released.

Podl’a navrhovaného spdsobu pripravy zosieteného lahčeného polypropylénu sa na tento účel použije t-butylperbenzoát v kombinácii s nenasýtenou zlúčeninou popísanou v predmete vynálezu, t-butylperbenzoát ako látka sieťujúca polypropylén pri tepelnom rozklade generuje dostatočné množstvo plynných produktov, potřebných pre vznik penovej átruktúry. V jednom stupni prebieha teda sieťovanie polyméru spolu s jeho 1’ahčením. Použitá nenasýtená zlúčenina zvyšuje účinnost sieťovanie a tým prispieva k modifikácii viskozity taveniny polypropylénu. Pri navrhovanom postupe 1’ahčenia polypropylénu nie je potřebný prídavok 9alšej látky (tak, ako v doteraz používaných postupoch) pre tvorbu plynov, nadúvajúcich polymérovú taveninu.According to the proposed process for preparing cross-linked bottled polypropylene, t-butyl perbenzoate is used for this purpose in combination with the unsaturated compound described in the present invention. Thus, in one step, the crosslinking of the polymer is carried out along with its 1 'twisting. The unsaturated compound used increases crosslinking efficiency and thus contributes to modifying the melt viscosity of the polypropylene. In the proposed polypropylene extrusion process 1, the addition of an additional 9 substance (as in the methods used hitherto) is not required for the formation of gases blowing the polymer melt.

Spdsobom pripravy zosieteného lahčeného polypropylénu podlá vynálezu možno získat produkt o objemovej hmotnosti až 1/12 z pdvodnej hmotnosti polypropylénu při rovnoměrněj velkosti uzavretých dutiniek. Riešenie spočívá v úpravě viskozity taveniny polypropylénu v priebehu jeho 1’ahčenia. Vynález umožňuje přípravu zosieteného lahčeného polypropylénu za použitia zníženého počtu reakčnýoh zložiek. Zosietením polypropylénu sa upravujú niektoré jeho fyzikálně vlastnosti, napr. odolnost voči rozpúštadlám, viskozita taveniny a niektoré pevnostné parametre.In the preparation of the crosslinked bottled polypropylene according to the invention, a product having a bulk density of up to 1/12 can be obtained from the original weight of polypropylene at a uniform size of the closed tubes. The solution consists in adjusting the melt viscosity of the polypropylene during its stretching. The invention allows the preparation of cross-linked bottled polypropylene using a reduced number of reactants. Crosslinking of polypropylene modifies some of its physical properties, e.g. solvent resistance, melt viscosity and some strength parameters.

Příklad 1Example 1

Do kadičky sa naváži 91 d práškového polypropylénu (TF 411 bez stabilizátora, výrobok n.p. Slovnaft), 3,5 d t-butylperbenzoátu, 5,5 d oC,co-akryl-(bis-etylénglykol)ftalátu (AEF) a zmes sa ddkladne zhomogenizuje. Potom sa medzi hliníkovými foliemi lisuje pri 443 K a tla ku 5 MPa 10 minút. Po uvolnění tlaku vznikne pěnový produkt a objemovou hmotnosťou 169 kg.nT\ Obsah gélu sa stanoví viacnásobnou extrakciou vriacim xylénom do konštantnej hmotnosti vzorky a v tomto případe je 10,7 %.Weigh into the beaker 91 d polypropylene powder (TF 411 without stabilizer, np Slovnaft product), 3,5 d t-butyl perbenzoate, 5,5 d oC, co-acrylic (bis-ethylene glycol) phthalate (AEF) and mix thoroughly homogenized. It is then compressed between aluminum foils at 443 K and 5 MPa for 10 minutes. Upon releasing the pressure, a foamed product was formed with a bulk density of 169 kg / l. The gel content was determined by multiple extraction with boiling xylene to a constant weight of the sample and in this case was 10.7%.

Příklad 2Example 2

Tak ako v příklade 1 sa sprecuje 94 d polypropylénu, 5 d t-butylperbenzoátu a 1 d AEF. Produkt má objemovú hmotnost 95 kg.m”^ a obsahuje 44,5 % gélu.As in Example 1, 94 d of polypropylene, 5 d of t-butyl perbenzoate and 1 d of AEF are treated. The product has a bulk density of 95 kg / m @ 2 and contains a gel of 44.5%.

Příklad 3Example 3

Zhomogenizuje sa 94,3 d polypropylénu, 5 d t-butylperbenzoátu a 0,7 d trietylénglykoldimetakrylátu. Zmes sa lisuje počas 7 minút pri teplote 453 K a tlaku 10 MPa. Vzniknutý 1’ahčený produkt obsahuje 53,6 % gélu a mé objemová hmotnost 306 kg.m“^.94.3 d of polypropylene, 5 d of t-butyl perbenzoate and 0.7 d of triethylene glycol dimethacrylate are homogenized. The mixture is pressed for 7 minutes at 453 K and 10 MPa. The resulting 1'lighted product contains 53.6% gel and my density is 306 kg.m ”^.

Příklad 4Example 4

Podl’a postupu ako v příklade 1 sa spracuje 92 d polypropylénu, 5 d t-butylperbenzoátu a 3 d AEF. Objemová hmotnoať 1’ahčeného polypropylénu je 76 kg.nT^ a obsah gélu 56,1 %.Following the procedure of Example 1, 92 d of polypropylene, 5 d of t-butyl perbenzoate and 3 d of AEF are treated. The bulk density of the expanded polypropylene is 76 kg / tonne and the gel content is 56.1%.

Příklad 5Example 5

Tu sa zhomogenizuje 87,5 d polypropylénu, 12 d t-butylperbenzoátu a 0,5 AEF. Po 5 min lisovaní pri 458 K a 7 MPa vznikne 1’ahčený produkt s obsahom gélu 74 % a objemovou hmotnos· tou 379 kg.m”3.Here, 87.5 d of polypropylene, 12 d of t-butyl perbenzoate and 0.5 AEF are homogenized. After 5 minutes of pressing at 458 K and 7 MPa, a 1-light product is obtained with a gel content of 74% and a bulk density of 379 kg / m 3.

Vo všetkých príkladoch vzniknutý 1’ahčený produkt mal jemnú rovnoměrná štruktáru uzavretých dutiniek, ktorých velkost sa pohybovala do 0,5 mm a bol bielej farby.In all the examples, the resulting lightweight product had a fine, uniform structure of closed tubes having a size of up to 0.5 mm and of white color.

Význam vynálezu spočívá v tom, že zosietený 1’ahČený polypropylén sa mfiže použiť na zvuková a tepelná izoláciu, ako obalový materiál pře křehké předměty s aplikáciou v automobilovém a stavebnom priemysle.The importance of the invention is that the crosslinked polypropylene can be used for acoustic and thermal insulation as a packaging material for fragile articles for application in the automotive and construction industries.

Příklad 6Example 6

Poatupom podlá příkladu 1 se spracuje 92 d polypropylénu, 4 <3 t-butylperbenzoátu a 4 d ot,oo -metakryl-(bis-propylénglykol)adipátu. Výsledkom je produkt s objemovou hmotnosťou 182 kg.m“3 s obsahom 67 % gélu.Following the procedure of Example 1, 92 d of polypropylene, 4- (3-t-butylperbenzoate) and 4 d of α-methacrylic (bis-propylene glycol) adipate are treated. The result is a product with a density of 182 kg / m 3 containing 67% gel.

Claims (1)

PREDMET VYNÁLEZUOBJECT OF THE INVENTION Spfisob přípravy zosieteného lahčeného polypropylénu, vyznačujůci sa tým, že sa k práškovému polypropylénu pri izbovej teplote primieša t-butylperbenzoát v koncentrácii 3 až 12 % hmot. a nenasýtená zlúčenina obecného vzorcaProcess for preparing cross-linked bottled polypropylene, characterized in that t-butyl perbenzoate is admixed to the powdered polypropylene at a concentration of 3 to 12% by weight. and an unsaturated compound of formula CH2 = C - C - 0 - (R1 - 0)n - (C - R2 - C - 0 -)m IEX - 0)n - C - C = 0¾CH 2 = C - C - 0 - (R 1 - 0) n - (C - R 2 - C - 0 -) m IE X - 0) n - C - C = 0¾ 0 0 0 o kde X je H alebo CH^, Rx je zbytok etylénglykolu alebo propylénglykolu, R2 je fenylén alebo zbytok alifatickéj dikarboxylovej kyseliny s počtom uhlíkov v reťazci 2 až 6, n mfiže nadobúdať hodnoty 1 až 3, m = O alebo 1, v koncentrácii 0,5 až 10 % hmot., zmes aa pri tlaku 1 až 20 MPa vyhřeje na teplotu 443 až 458 K a tlak sa uvol’ní.Where X is H or CH 2, R x is a ethylene glycol or propylene glycol radical, R 2 is phenylene or an aliphatic dicarboxylic acid radical having a number of carbons in the chain of 2 to 6, n being 1 to 3, m = 0 or 1, at a concentration of 0.5 to 10% by weight, the mixture aa is heated to a temperature of 443 to 458 K at a pressure of 1 to 20 MPa and the pressure is released.
CS793278A 1978-12-01 1978-12-01 Process for preparing crosslinked foamed polypropylene CS201871B1 (en)

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