. i s a s peci ?ca ti on.

' UNITED S TA TES , PA TENT cl a r i on.

LEO H . BA EKELA ND, 0 F _ . Y ONKEBS , NEW v Y OR K.
ms r non or MA KING INS OLUBLE r a onu c' r s or r r r eu on A ND ' r onmnnmr ,
9 4 2 , 6 9 0 .
No Dr a wi ng. - ' .
To a l l whom i t ma y concer n:
l l e i t known tha t 1 , Leo II. Ba r nes / mo,
a ci ti z en of the Umtcd S ta tes , r es i di ng a t.
S nu g l l ock, , . ' l l a r mony l a r l c, Y onker s , i n
the cou nty of \ \ " es tches ter a nd S ta te of New
Y or k, ha v e i nv ented cer ta i n new a nd u s ef u l .
l mpr ov emeu ts - i n Methods of Ma ki ng l i t-
s ol u b l e C ondens a ti on l r odu cts ' ot l henol s
a ml l t or ma l dchj yde, of whi ch the f ol l owi ng
i n my pr i or a ppl i ca ti on S er f No . 3 5 8 , 1 5 6 ,
i i l ed l t eb r u a r y l b , 1 9 0 ?, l ha v e des cr i b ed
a nd cl a i med a method of i ndu r a ti ng, r l i b r ou s
or cel l u l a r . ma ter i a l s whi ch cons i s ts i n i m
pr egna ti ng or mi x i ng them wi tha phenol i c
b ody a nd f or ma l dehyde, a nd ca u s i ng the
s a me to r ea ct. wi thi n the b ody of the ma te
r i a l to yi el d a n i ns ol u b l e i u du r a ti ng con
' dens a ti on J n' otl nct, the r ea cti on b ei ng a ccel
es n' cd b y the u s e of hea t or con. .
er u tcd i t
( l ens i ng a gents . i n the cou r s e of thi s r e
a cti on cons i der a b l e q u a nti ti es of wa ter a r e
pr odu ced, a nd a dr yi ng oper a ti on i s r es or ted
to to ex pel i t. - _ _ -
The pr es ent. i nr eu ti on r el a tes toi the pr o
du cti on of ha r d, i ns ol u b l e a nd i nf u s i b l e con
dens a ti on pr odu cts of phenol s a nd f or ma l
dehyde. ' -
l n pr a cti ci ng the i nv enti on 1 - r ea ct u pon.
a phenol i c b ody wi th f or ma l dehyde to ob
ta i n a r ea cti on n' odnct whi ch i s ca pa b l e of
tr a ns f or nmti on y hea t i nto a n i ns ol u b l e a nd
i n f u s i b l e b ody, a nd then conv er t thi s r ea c
ti on pr odu ct, ei ther a l one or compou nded
wi th a s u i ta b l e l i l l i ng ma ter i a l , i nto s u ch i n
s ol u b l e a nd i nl ' u s i b l c b ody b y the comb i ned
a cti on of hea t a nd pr es s u r e. Pr ef er a b l y
the wa ter pr odu ced du r i ng the r ea cti on or
a dded wi th the r ea cti ng b odi es i s s epa r a ted
b ef or e ha r deni ng the r ea cti on pr odu ct. By
pr occedi mr i n thi s ma nner a mor e compl ete
contr ol of t- hc r ea cti on i s s ecu r ed a nd other
i mpor ta nt a dv a nta ges a r e a tta i ned a s her e
i na f ter s et f or th. '
~ If a mi x tu r e of phenol or i ts homol ognes
a nd f or ma l dehyde or i ts pol ymer s b e hea t;
ed, a l one or i n pr es ence 0 ca ta l yti c or con
dens i ng a gents , the f or ma l dehyde b ei ng
pr es ent i n a b ou t the mol ecu l a r pr opor ti on
r eq u i r ed f or the r ea cti on or i n ex ces s ther e
of , tha t i s to s a y, a ppr ox i ma tel y eq u a l v ol
u mes of commer ci a l phenol or cr es yl i c a ci d
a nd commer ci a l f or ma l dehyde, thes e b odi es
r ea ct u pon ea ch other a nd yi el d a pr odu ct
cons i s ti ng of two l i q u i ds whi ch wi l l s op
_ Bpeetne' a tl oa 0 1 Letter s Ea ten- t. I : I a tentcd Dec. ' 7 ' , 1 9 0 9 .
A ppl i ca ti on ?l ed J u l y 1 : , 1 9 0 7 , S er i a l no. . a a a m. _ '
a r a te or s tr a ti f on s ta ndi ng. ' The l i ghter
or s u per na ta nt i q u i d i s a n a q u eou s s ol u ti on,
whi ch conta i ns v the wa ter r es u l ti ng f r om the
r ea cti on or a dded wi th the r ea gents , wher e
a s the hea v i cr l i q ni d i s oi l y or v i s cou s i n.
cha r a cter a nd conta i ns the ti r ' s t pr odu cts of
chemi ca l condens a ti on or dehydr a ti on. The
l i q u i ds a r e r ea di l y s epa r a ted, a nd the a q u c-
ou s s ol u ti on ma y b e r ej ected or the wa ter
ma y b e el i mi na ted b y eya por a ti on. ' l ' he
oi l y l i q u i d ob ta i ned a s a b ov e' des cr i b ed i s
f ou nd to b e s ol u b l e i n or mi s ci b l e wi th a l co~
hol , a cetone, ) henol a nd s i mi l a r s ol v ents or
mi x tu r es of the s a me. Thi s oi l y l i q u i d ma y
b e f u r ther s u b mi tted to hea t: on a wa ter - or
s tea m- b a th s o a s to thi cken i t s l i chtl y a nd
to dr i v e otl ' a ny wa ter whi ch mi g i t s ti l l b e
mi x ed wi th' i t. If the r ea cti on b e per mi tted
to pr oceed f u r ther the condens a ti on pr odu ct
ma y a cq u i r e ' a mor e v i s cou s cha r a cter , b e
comi ng gel a ti nou s , or s emi - pl a s ti c i n con-
s i s tcnce; " l ' hi s a nodi ?mti on of the' r odu ct
i s i ns ol u b l e or i ncompl etel y s ol u b l e 1 n a l co
hol b u t s ol u b l e or pa r ti a l l y s ol u b l e i n a ce
tone or i n a mi x tu r e of a cetone a nd a l cohol .
_ The condens a ti on pr odu ct ha v i ng ei ther
the oi l y or s emi - pl a s ti c cha r a cter ma y b e
s u b j ected to f u r thcr tr ea tment a s her ei na f ter
' dcs cr i b ed. - By hea ti ng the s a i d condens a
ti on pr odu ct i t i s f ou nd to b e tr a ns f or med
i nto a . ha r db ody, u na f f ected b y moi s tu r e,
i ns ol u b l e i n a l cohol a nd a cetone, i nf u s i b l e,
a nd r es i s ta nt to a ci ds , a l ku l i es a nd a l mos t
a l l or di na r y r ea gents . Thi s pr odu ct ~ i s
f ou nd to b e s u i ta b l e f or ma ny pu r pos es , a nd
ma y b e empl oyed ei ther a l one or m a dmi x -
' tu r e wi th other s ol i d, s cmr hq md or 1 1 u i d
ma ter i a l s , a s f or i ns ta nce a s b es tos 6 r ,
wood ?b er , other ?b r ou s or _ cel l u l a r ma te
r i a l s , r u b b er , ca s ei n, l a mp b l a ck, mi ca , mi n-
er a l powder s a s z i nc ox i d, b a r i u m s u l f a te,
' etc. , pi gments , dyes , ni tr ocel l u l os e, a b r a s i v e
ma ter i a l s , l i me, s u l f a te of ca l ci u m, gr a phi te,
cement, powder ed ' hor n or b one, pu mi ce
s tone, ta l cu m, s ta r ch, col ophonnu n, r es i ns or
7 0
7 5
8 0
9 0
9 5
1 0 0
gu ms , s l a te du s t, etc. , i n a ccor da nce wi th the '
pa r ti cu l a r u s es f or whi ch i t i s i ntended, a nd
i n mu ch the s a me ma nner a s i ndi a r u b b er i s
compou nded wi th the a b ov e- na med a nd
other ma ter i a l s to yi el d v a r i ou s v a l u a b l e
' pr odu cts . - In compou ndi ng the condens a
ti on or dehydr a ti on pr odu ct i n thi s ma nner ,
the des i r ed ma ter i a l s a r e mi x ed wi th the
s a me b ef or e s u b mi tti ng. i t to the ?na l ha r
deni ng oper a ti on b el ow des cr i b ed.
1 1 0
1 0
. 1 5
2 0
2 5
3 5
4 0
Q .
In or der to conv er t the condens a ti on or
dehydr a ti on- pr odu ct i nto the ?na l pr odu ct
a b ov e- des cr i b ed I ma y s u b j ect i t toa tem
per a tu r e whi ch wi l l depend u pon the s pe
ci ti c r es u l ts s ou ght. If i t b e des i r ed ' to mol d
the ma ter i a l di r ectl y the condens a ti on pr od
u ct i s pou r ed or pr es s ed i nto a s u i ta b l e mol d
a nd i s s u b mi tted ther ei n whi l e ma i nta i ni ng
a ppr opr i a te pr es s u r e to a s u i ta b l e tei n ) er
a tu r e, s a y a b ou t 1 1 0 - 1 4 0 " 0 . ; u nder thes e
condi ti ons ther e i s ob ta i ned i n f r om one to
two hou r s or l es s a ha r d, compa ct, per f ectl y
homogeneou s ma s s s i mi l a r i n i ts pr oper ti es
to ha r d r u b b er or to i v or y, i ns ol u b l e i n a l co- _
hol , a cetone, a nd r es i s ta nt to hea t or i nf u s i
b l e, a nd r es i s ta nt to moi s tu r e a nd mos t
chemi ca l r ea gents a s a b ov e des cr i b ed. In
ca s e the- ) r odu ct b e. ?r s t mi x ed wi th a s b es tos .
l i b er , r u b er , powder ed s u b s ta nces or other
ma ter i a l s a s a b ov e des cr i b ed, a nd hea t b e
ther ea f ter a ppl i ed a v compou nd i s ob ta i ned
i i i - the f or m of ha r d ma s s es conta i ni ng the
i ns ol u b l e condens a ti on pr odu ct des cr i b ed.
S u ch ma s s es ma y b e pr odu ced di r ectl y i n
a ny des i r ed f or m b y the u s e of a s u i ta b l e
mol d, or they ma y b e pr odu ced . i i i a b l ock or
i r r egu l a r ma s s whi ch ma y b e cu t, s a wed,
tu r ned or other wi s e ma ni pu l a ted to a ny
s u i ta b l e f or m or s i z e. '
S ma l l pr o or ti ons of s ol v ents ma y b e
a dded to the i ni ti a l condens a ti on pr odu ct i n
or der to f a ci l i ta te the compou ndi ng or mi x
i ng of the s a me, the r es u l ti ng mi x tu r e b ei ng
then s u b mi tted to the f i na l b a ki ng or ha r
deni nor pr oces s a s des cr i b ed. -
Whi l e I ha v e i ndi ca ted a b ov e a pr a cti ca l
ha r deni ng temper a tu r e of 1 1 0 1 4 0 C . i t
s hou l d b e u nder s tood tha t hi gher temper
a tu r es ma y b e empl oyed, i n whi ch ca s e the
ti me r eq u i r ed f or the ha r deni nw pr oces s i s
cons i der a b l y r edu ced; the ha r deni ng ma y
a l s o b e condu cted a t 1 0 0 C . a nd ev en a t
4 5
s o
5 5
6 0
6 5
l ower temper a tu r es , mor epa r ti cu l a r l y f or
i mpr egna ti ng ?b r ou s or i ce l u l a r ma ter i a l s ,
b u t i n thi s ca s e the ha r deni ng i s f ou nd to
b e v er y s l ow a nd s ome da ys ma y b e r eq u i r ed
f or i ts compl eti on. The ha r deni ng ma y b e
gr ea tl y a ccel er a ted b y a ddi ng s ma l l pr opor
ti ons of ca ta l yti c. a gents , or s o- ea l l ed con
dens i ng a gents , a s f or i ns ta neez i nc chl or i d,
other meta l l i c chl or i ds , a ci ds or s a l ts . In
ca s e s u ch condens i ng a gents a r e a dded the
ha r deni ng occu r s r a pi dl y a t r el a ti v el y l ow
temper a tu r es .
The mode of a ppl i ca ti on or compou ndi ng
of the condens a ti on pr odu ct wi l l of cou r s e
depend u pon the r es u l ts s ou ght. It or tr ea t
i ng or i ndu r a ti ng wood, the s u r f a ce onl y
ma y b e tr ea ted, or i t ma y b e tr ea ted
thr ou ghou t i ts ma s s s u b s ta nti a l l y a s de
s cr i b ed i n my copendi ne a ppl i ca ti on a b ov e
r ef er r ed to; the tr ea ted ma ter i a l i s ther e
a f ter s u b mi tted to hea t, s ome condens i ng
a gent b ei ng a dded i f des i r ed. F or f a ci l i ta t
i ng the penetr a ti on of wood or the l i ke the
9 4 2 , 6 9 9
condens a ti on pr odu ct ma y b e s l i ghtl y hea ted
to r ender i t mor e ' mob i l e, or s ma l l i r opor
ti ons of s u i ta b l e s ol v ents ma y b e a dded.
- The l i na l hea ti ng or b a ki ng b y whi ch the
condens a ti on pr odu ct, a l one or compou nded,
i s conv er ted i nto , a n i ns ol u b l e b ody s hou l d
b e etl ected i n a cl os ed v es s el i n ca s e the tem
per a tu r e ex ceed 9 0 - 1 0 0 0 . ; wi thou t thi s
n- eca u ti ou . v a por s of f or ma l dehyde a nd the
l i ke es ca pe ca u s i ng f oa m a nd a i r b u b b l es ;
f u r ther mor e thel os s of the r ea gents a nd the
di s tu r b a nce of the pr opor ti ons b et ween then' i
) r ev ents ob ta i ni ng a pr odu ct of ma x i mu m
ha r dnes s a nd u ni f or m tex tu r e. i n a cl os ed
v es s el u nder pr es s u r e the ( mer a ti ou pr oceeds
wi th pr eci s i on, a nd a u ni f or m r es u l t ma y b e
a l wa ys ob ta i ned. . ' _
Ins tea d of or di na r y phenol I ma y u s e cr e
~ s ol a nd i ts homol ogou s , - or other phenol i c
b odi es . If des i r ed I ma y empl oy i n pl a ce of
commer ci a l f or i mi hl ehyde a s ol u ti on of a n
hydr ou s f or ma l dehyde i n phenol , or the
" pol ymer of f or ma l dehyde whi ch on hea ti ng
s pl i ts u p i nto a nhydr ou s f or ma l dehyde, ma y
b e u s ed. 1 _
The i ni ti a l oi l y, v i s cou s or s emi - pl a s ti c
condens a ti on pr odu ct. ma y b e ob ta i ned v i n
7 0
9 0
v a r i ou s wa ys , a s f or i ns ta nce b y dggcs ti nv ~ a '
s u i ta b l e mi x tu r e of phenol a nd or ma l e
hyde i n a n a u tocl a v e, or mer el y b y b oi l i ng
a mi x tu r e of the s a me i n a n open' v es s el pr o
v i ded wi th a r etu r n condens er i n or der to
a v oi d l os s a nd v a r i a ti on of _ pr opor ti ons .
. v er y s ma l l pr opor ti on of mi ner a l or or ga ni c
a ci d, or of z i nc chl or i d, ca l ci u m chl or i d, or
other s a l t or a gent f a v or i ng condens a ti on
ma y b e a dded to the mi x tu r e, the pr opor ti on
b ei ng- i n a l l ca s es s o s ma l l a s to a v oi d s u ch
ener geti c r ea cti on a s wi l l not per mi t the i i i
ter ni edi a te oi l y, v i s cou s or s emi - pl a s ti c con
dens a ti on i r odu ct to b e ob ta i ned. Or I ma y
a dd a s ol i d s a l t a s f or i ns ta nce ca l ci u m chl o
r i d to the mi x tu r e of phenol a nd f or ma l de
hyde i n whi ch ca s e the ca l ci u m chl or i d i m
medi a tel y a b s or b s wa ter a nd f or ms two di s - '
ti nct l a yer s , the l ower one b ei ng f or med b y a
v er y dens e a q u eou s s ol u ti on of ca l ci u m chl o
1 0 0
1 0 5
r i d, the u pper one b y the dehydr a ted i ni x - .
tu r e.
I cl a i m: '
1 . ' l i e method of pr odu ci ng a ha r d, coni
pa ct, i ns ol u b l e a nd i u tu s i b l e condens a ti on
pr odu ct of phenol s a nd f or ma l dehyde, whi ch
cons i s ts i n r ea cti ng u pon a phenol i c b ody
wi th f or ma l dehyde, a nd then conv er ti ng' the
. r odu ct i nto a i a r d, i ns ol u b l ea nd i nf u s i b l e
Body b y the comb i ned a cti on. of hea t a nd
pr es s u r e. _ ' '
2 . The method of ma ki ng a r ti cl es conta i n
i ng a n i ns ol u b l e a nd i ntu s i b l c condens a ti on _
pr odu ct of phenol s a nd f or ma l dehyde, whi ch
cons i s ts i n r ea cti ng on a phenol i c b ody wi th
f or ma l dehyde, pr odu ci ng ther eb y a r ea cti on
r odu ct ca pa b l e of tr a ns f or ma ti on b y hea t.
i nto a n i ns ol u b l e a nd- i nf u s i b l e b ody, f or m
1 1 5
1 2 0
_ . i ng the a r ti cl e f r om s a i d r ea cti on pr odu ct,
- 9 4 2 , 6 9 9
i ng the a r ti cl e f r om s a i d r ea cti on pr odu ct,
a nd r ender i ng the a r ti cl e ha r d, i ns ol u b l e a nd
i nf u s i b l ' e b y a ppl i ca ti on of hea t a nd pr es
s u r e. ' ' _ -
3 . The method of ma ki ng a r ti cl es conta i n
i ng a n i ns ol u b l e a nd i u f u s i b l e coml ens a ti on
pr odu ct of phenol s a nd f or ma l dehyde, whi ch
cons i s ts ' i n r ea cti ng on a - phenol i c b ody wi th
f or ma l dehyde, pr tu l u ci n; r ther eb y a r ca cti on
n' odu ct ca pa b l e of tr a ns f or ma ti on b y hea t
l l l l O a n i ns ol u b l e a nd i nf u s i b l c b ody, s epa r a t
i ng i ' a ter f r om the r es u l ti ng pr odu ct, f or m
a nd r ender i ng the a r ti cl e ha r d, i ns ol u b l e a nd
i nf u s i b l e b y a ppl i ca ti on of hea t a nd pr cs - .
s u r e. .
. ~ l . The method of ma ki ng a r ti cl es conta i n
i u g a n i ns ol u b l e a nd i nf u s i b l e condens a ti on 1
pr odu ct. of phenol s a nd f or ma l dehyde, whi ch !
' mns l s ts i n r ea cti ng on a phenol l C b ody wi th
f or ma l dehyde, pr odu cmgther eb y a r ea cti on
8
pr odu ct ca pa b l e of tr a ns f or ma ti on b y- hea t
i nto a n i ns ol u b l e a nd i nf ns i b l e b ody, f or m
i ng the a r ti cl e f r om s a i d r ea cti on pr odu ct .
compou nded wi th a ' ti l ti ng ma ter i a l , a nd r en- '
der i ng the a r ti cl e ha r d, i ns ol u b l e a nd i nf u s i
b l eb y a ppl i ca ti on of hea t a nd pr es s u r e.
. 7 5 . Ina method of ma ki ng a r ti cl es cou ta i n
i ncr a n i ns ol u b l e a nd i nf u s i b l e coi u l ens a ti on
pr odu ct of phenol s a nd f or ma l dehyde, the
s tep_ whi ch cons i s ts i n ca u s i ng the wa ter to
s epa r a te f r om the mi x tu r e of a phenol i c b ody
a nd a n a q u eou s s ol u ti on of f or ma l dehyde b y
a ddi ng to s a i d mi x tu r e a meta l l i c s a l t s ol u b l e
i n wa ter a nd a da pted to ca u s e s u ch s epa r a
ti on. ' ' ' i
. l n tes ti mony wher eof , I a l l i x a ny s i gna tu r e
i n pr es ence of t\ ' q wi tnes s es . ,
' LEO 1 L BA EKELA ND.
Wi tnes s es : , . _ _
' F a ce R . C a ner ,
l l a ma S . Ta i wa n!