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3,370,020
PROCESS FOR THE PRODUCTION OF PHOSPHO
NITRILIC POLYMERS AND POLYMERS PRO
DUCED THEREBY
3,370,020
15
20
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peratures.
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40
45
50
60
65
resistant.
3,370,020
M(OR):
calcium chloromethoxide,
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60
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include
sodium methoxide,
sodium octyloxide,
lithium methoxide,
lithium octyloxide,
potassium methoxide,
potassium octyloxide,
magnesium methoxide,
magnesium octyloxide,
calcium methoxide,
calcium octyloxide,
sodium phenoxide,
sodium-1-naphthoxide,
lithium phenoxide,
lithium-1-napthoxide,
magnesium phenoxide,
magnesium-2-naphthoxide,
potassium phenoxide,
potassium-2-naphthoxide,
calcium phenoxide,
calcium-1-naphthoxide,
sodium chloromethoxide,
sodium o-, m- or p-chlorophenoxide,
lithium chloromethoxide,
lithium o-, m- or p-chlorophenoxide,
potassium chloromethoxide,
potassium,
o-, m- or p-chlorophenoxide,
magnesium-6-iodo-2-naphthoxide,
sodium bromomethoxide,
sodium iodomethoxide,
magnesium fluoromethoxide,
potassium-2-bromoethoxide,
lithium-2-iodopentoxide,
calcium-7-fluorooctyloxide,
sodium nitromethoxide,
Sodium-8-nitrooctyloxide,
lithium o-, m- or p-nitrophenoxide,
calcium-3-nitro-1-naphthoxide,
potassium cyanomethoxide,
magnesium-4-cyanohexoxide,
lithium methoxymethoxide,
Sodium o-, m- or p-nitrophenoxide,
lithium-2-cyano-1-naphthoxide,
magnesium o-, m- or p-cyanotolyloxide,
calcium-3-fluoroxyloxide,
magnesium o-, m- or p-n-butoxyphenoxide,
sodium-3-t-butoxyoctyloxide,
calcium phenoxymethoxide,
Sodium o-, m- or p-phenoxyphenoxide,
calcium-3-phenoxy-1-naphthoxide,
lithium-2-napthoxyethoxide,
sodium ethoxide,
sodium-1,1,1-trifluoroethoxide,
sodium-1,1,1,2,2-pentafluoropropoxide,
calcium ethoxide,
lithium propoxide,
potassium n-butoxide,
potassium o-, m- or p-methoxyphenoxide,
sodium o-, m- or p-benzyloxide, and the like.
The second Step of our novel process results in the
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3,370,020
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65
70
75
3,370,020
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is then added dropwise over 3 hours to the solution of
phosphonitrilic chloride polymer mixture. The resulting
mixture is then stirred and refluxed for 3 days, during
which time a white precipitate of sodium chloride is
formed. Tetrahydrofuran is removed by distillation. When
the mixture becomes excessively viscous, dry benzene is
8
1000 parts and precipitated dropwise into 5000 parts of
heptane mixture.
alkali metal and alkaline earth metal compounds are 30 eric mixture with water at about 100 C., hydrolysis re
reacted with various polymer mixtures produced as desults.
EXAMPLE 2.0
mer mixtures are set forth in Table I below. The conditions of polymerization and esterification are also varied
(Comparative)
parative
in each example.
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TABLE I
Polymerization Conditions
Esterification Conditions
--
Ex.
Temp.,
C.
per
Ex. No.1
250
4
i.
260
2
1
220
16
1.
230
8
3
245
5
1
300
%
3
200
48
1
210
24
1.
240
6
1
250
3%
3
280
1.
i
235
8
1
235
8
3
260
4
3
1 Polymerization termination.
C.
200
175
150
125
60
25
160
85
75
40
75
100
150
200
Precip. Agts.
Time,
M0R.
3
5
8
12
48
168
6
24
5
96
30
16
8
3
hr.
(Comparative)
60
65
TI)
H2O
Per
(Non-Solvents) cent 3
Per-
Air
N2
C. Effect M.W.
cent
Tiethyl ether_ _
Benzene-------n-Heptane. -------do-- - - -do
----doDiethyl
n-Heptane ----- - - -do-------------do---------- - - -do.--------- - - -do---------JDiethyl ether-----do----------
400
410
405
400
390
420
410
400
380
400
425
415
400
375
440
425
420
425
415
450
430
430
400
410
440
425
420
400
100
150.
120
215
60
240
230
215
220
90
240
200
260
235
32
35
28
39
41
27
33
31
26
35
37
28
30
31
S.P.,
None- 80,000
--do -- 90,000
--do -- 75,000
--do -- 77,000
--do -- 70,000
--do -- 100,000
--do -- 85,000
--do -- 82,000
--do -- 67,000
--do-- 70,000
--do-- 89,000
--do-- 81,000
--do -- 77,000
--do -- 65,000
C} 3
0
0
0
0
0
0
0
0
0
0
0
0
0
0
70
75
3,370,020
about 100 C.
We claim:
10.
References Cited
UNITED STATES PATENTS
20
10
2,214,769
3,194,787
3,271,330
878,324
30