DE1468822A1 - Stabilized methyl chloroform compositions - Google Patents

Description

Dr. Walter Beil

Dr. Hans Joadilm WoM

Hans Chr. Beii ■ ■; ' ■ '

- lawyers

Frankfurt a. M. ~ Hädist

Adelooatrafie 58 Telephone 301 034, 3ttiO25

Our ir. 11 842 '

Pittsburgh Plate Glass Company Pittsburgh, Pa., Y.St.A.,

Stabilized liethylehloroforia compositions

The invention relates to; cetylenically unsaturated and / or saturated ^ all pha ti see monohydric alcohols with up to 8 carbon atoms and an ifitroalkane with 1 to 5 carbon atoms stabilized methyl chloroform compositions whose evaporation properties by the addition of 0.05 ^; to 5jO G-ew./έ iEoluol are improved. - -

kethylcliloroform or 1,1,1-irichloroethane, a norm flitsfci <; the chlorinated hydrocarbon, is an important one technical solvent, but because of its applicability his inclination to become involved in the practice, in particular with The contact between all areas to be replaced is limited.

Lan'-has berö-it's' proposed a series of connections, which is added to the Met; h7! chloroform alone or in a "combination" should be grounded in order to give it stability, e.g. also alcohols. For example, the Ii S patent document 2 811 252 Ixethylcliloroformzusa · men-sationen described, the smaller Amounts of non-primary alkanols with 4 to 8 carbon atoms;

men included. Methyl chloroform compositions with a ^

ü-ehcilt CiXL acetylenioch unsaturated monohydric alcohols ψ-

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ν ..? _f .. _s ,, U & V® documents BAD ORIGfNAi.

with fewer than 8 carbon atoms are explained in the Ub "patent document 2 ' 338 458. The' LS patent document 3 000 978 shows that tert. butylalcohol can improve the stability of lietin / chloroform Finally, in 3 070 634 it is pointed out that ketlrylchlorofoiTazusanmensetzun ^ s, which contain both acetylenically unsaturated monohydric alcohols and saturated alcohols, have improved stability properties.

Those resulting from the use of monohydric alcohols " advantageous properties of the 'Heth'ylchloroformzusaiamenset., un. ^ en are however "at the same time as a disadvantage connected, hethyTchloroforriizusaruiüensetzüngen, " which contain a monohydric alcohol, from a liientporous. Surface, e.g. of an ietalloberfiär.; He, "verdi ^ ipft, Thus, even with very low concentrations of only 0.75 G-ev./J alcohol, sticks remain on this surface. Such pitting occurs in the absence of alcohols not on.

It has now been found that this pulpit can be overcome in this way lets you do the alcoholic -msaniiaensetzun a small amount of toluene adds o.ie the dar ^ pftin ^ s properties the ethylchloroform addition is essential improved and a.leckenpbildung a.ussc'nlosc'n.

An advantageous '.-. Iriaing% ^r i.rd with loluolicon concentrations of about 0.05 to 5 G-ev / ..', based on the keth. 0.25 to .etv / a .3.0 G-ev /./ ^; j, based on the Meth§rlchlorofori, i, are used. Even higher concentrations (up to ... IG ^ ev-.o ) ^ ,, are .. applicable, but economically uiivprteiL] Lh; -ft. _v ., - v .. ^., ... _: - .r "

Da.s toluene can erfindun ^ convention under, iecer with alcohol .stabil _-.!; "Sieren i-iethylchloroforiiausaii.i.iensetzun ^ j ä..h. .Each Hetli 1-

, ^f

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chloroform composition are added to improve their stability, reduce corrosion, etc., ^r . is mixed with one or more alcohols, namely monohydric aliphatic saturated and unsaturated alcohols, as they are described in the literature cited above. Most of these alcohols contain no more than 8 carbon atoms and usually at least 4 carbon atoms. Butyl alcohol, sec. Butyl alcohol, isobutyl alcohol, tert. Amyl alcohol, 2-octanol and the like are saturated monohydric alkanols which are particularly suitable for this purpose 3-butyn-2-ol, 3-methyl-1-pentyn-3-ol, 2-methyl-1-ol, 2-methyl-3-hexyn-2-ol and propargyl alcohol should be mentioned.

Depending on which stabilizing! Function the alcohol or the alcohol mixture should have or whether other stabilizing If additives are present, the alcohol concentration in the methyl chloroform can vary considerably. Rarely the alcohol content of the methyl chloroform is lower than 0, Oi? öew.y ^. Usually between 0.5 and 5.0 G-ew. '/ Ö (mostly 1.0 to 2.0 Gev /./ s), based on the kethylehloroform, is used. Higher concentrations are useful, but rarely used.

In the present case, the toluene content is usually 50 to 500 G-ev. '; J, based on the alcohol content. A erfinäungsgeraäSe KethylchloroxOrJitzusai.ii ^ eiisetzung contains, for example about ÖIE half or twice the weight of the alcohol or of the ArKoholßei ^ ischs of toluene "Substituting for example äem Methylcfcloroform Alicohol in a Hen ^ e of T wt. ^ To, so is & Kenge X2 of added Soluols usually, between 0.5 and 5.0 wt - _r i based: .uf the Methylclilorofoiia..

BATH

The addition of toluene according to the invention extends, as mentioned; not only on methyl chloroform compositions containing alcohols, but also on compositions that contain other additives to stabilize the methylchloroform or prevention of corrosion.

In such compositions, nitroalkanes, especially nitroalkanes with 1 to 3 carbon atoms, such as liitromethane, Litroethane, a-jüitropropane, ß-xiitropropane or 2-chloro-nitroathane be included.

In addition, epoxies with 2 "to 10 carbon atoms, such as ethylene oxide, propylene oxide, 2-methyl-1,2-epoxypropane, epichlorohydrin, styrene oxide, glycidol, Amylenox3-d, 1,2-epox3- ^r octane, epoxycyclopenten, Ci ^ clohexenox ^ d, butylene oxide with the exception of diepoxides, v / ie butadiene dioxide, .d and Cj ^ clopentaöien- ■ diepoxyd, be present.

Also bioxolane (1,3-dioxolane) or substituted 1,5-dioxolane, how . 2-ethyl-1,3-dioxolane, 2-ethyl-7,3-dioxolane, 2-isopropyldioxolane, 2,2-J) imethyl-1,3-Ä.ioxclsii, 2-lietliyl-4-methyl-1,3-dioxolane ,. 5,5-dimethyl-1,3-dioxolane, 2-chloro-4-methyl-1,3-dioxolane can be included, as well as dioxane, tetrahydrofuran, JTux'an, pyran and other cyclic compounds as well as ketones, liitrile and i) ialI'_oxyE.lka.ne.

The invention is useful; I apply you to solution solutions in which the ethyl chloroform is not a basic solvent, but one of several solvents, e.g. Call solvent solutions from methyl chloroform in terbindun ?; with a; .- η or more other chlorinated ^ ohlenv / asserstofflösun / sßiitteln, v IU MethylenchlorlcL, Tetrr-chloriiohlenstofi ', 1,2-j) ichlor length than' richloräthylen- and P-erchlor-.Ithyleii!.

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Specific Iiäsungsmittelgemisehe this type contain 70-85 Λ Hethylchlorofarni and 50-15 üew.ya Perchloräthylenj 70-95 wt. / O methyl chloroform and 50-5 Gew./ "1.2-1) 1 or the like chi than or 65-95 wt .> £ methyl chloroform and 55-5% by weight of irichlorethylene.

The fol _& end examples serve to illustrate the invention.

example 1

ßs vAirde a Methylchlorofor'.Composition made with the following ingredients:

Addition weight # _f based on

Methyl chloroform tert. Butyl alcohol 2.0 ifitromethane 2.0 tert. Amyl alcohol 1.0 iutylene oxide 0.5 Dimethoxyethane 0.2

These susaitimings are given in the l'ahelle I. Amounts of ioluene added. Then the TerdaDvpxun & Söeschwiiidiv-lcoit of the various compositions determined by adding 2 ecm each of the compositions with the pipette in a notch in the middle of a small Stainless steel plate filled. And the time found pis all the solvent had evaporated.

The compositions examined are shown in Table 1 above and the results obtained with them are listed:,

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Table I.

additive Percentage by volume, related 2 Digestion time, ; found on Keth, y! chloroform Kirmtenj 16:37 none _ 16:35 11:58 toluene 2.0 11:52 11:05 toluene 3.0 11:05 10 * 44 toluene 5.0 10:32 example

Ss became a methyl chloroform composition having the following Components manufactured:

additive

tert. But.y! Alcohol i'fitromethane Isobutyl alcohol Butylenoxj'd 2-methyl-3-iutin-2-ol

Wt. ¹ ;: /, based on
Kethylchlorox'orm

2, 0 2, 0 1, 0 O, 5 O, 5

The small amounts of toluene listed in Table II were added to this composition. Subsequently., The '
Evaporation rate of the various. Compositions determined by the method described in Example 1: _;

additive

none toluene tolupl tolupi.

Table II

Percentage by volume, based on Hethylchlo roform

Evaporation time,;. i-iinu ten: seconds '

.. 20: 5 _; 6 .... 2Q; Q4
_r ', 10: 44l' ^ p: A4,. '. ./

10:46. "Jp

8:14 "a: J4

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The results obtained show that even the addition of small amounts of toluene to an alcohol-containing methyl chloroform composition the rate of evaporation of this composition is significantly reduced.

Example 3

Samples of the basic composition of Example 2 were made

A with 5 wt. $ Toluene

B with 5% by weight η-hexane and

C with 5 wt. ^ Cyclohexane

offset. The rate of evaporation was then set of the various compositions according to the method of Example 1. Those listed in Table III Results from 4 experiments show. that neither n-hexane nor cyclohexane has a noticeable effect on the rate of evaporation the methyl chloroform composition, while toluene the evaporation rate of the alcohol-containing composition significantly reduces.

Table III

Composition Evaporation Time Through-

Minutes: seconds cut

A 20:24} -17:09; 18: 16 * 18:42 18s38

B 5:22} 6:03} 7:14; 6:56 6:24

C 19:16; 16:07} 16:50; 16:08 17:05

B 17: 1Of 17:14} 19 * 57} 18:20 T8: 00

Example 4

The methyl chloroform compositions described in the examples vmrden also checked whether they at residue from evaporation from a polished metal plate. For this purpose, the solvent preparations were made on the long side of a polished 20.3-2 χ 91 »4 cm Aluiiiiniuiaplatte poured, which one in a kinkel of about

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Held 45 °. The 3usa compositions were then allowed to evaporate from the surface.

The compositions containing no toluene dissolved visible residues (stains) on the plate.

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ORIÖfNAL INSPECTED

Claims (3)

Claims Kit acetyleniscli unsaturated and / or saturated aliphatic Monohydric alcohols stabilized methylchloroform compositions, known thereby draws that they contain Soluol as a further additive. 2. Stabilized methyl chloroform compositions after
Claim 1, characterized in that they are related
on the diethylchloroform, 0.05 to 5> 0. Contains 7a by weight of loluene. 3. Stabilized methyl chloroform compositions after
Claims 1 and 2, characterized in that, based on the methyl chloroform, they contain 0.05 to 5.0 weight w / u aliphatic monohydric alcohol and 0.5 to 5 »0 weight w / w toluene. Pittsburgh Plate Glass Company
Pittsburgh, Pa., T.St.A. Right 809901/0858