Foshan Dragon Edge Outdoor Equipment Co., Ltd , https://www.dragon-edge.com
Method for preparing cresol black medicine
The cresol black drug is formed by the action of cresol and phosphorus pentasulfide . The reaction formula is as follows:
The synthesis conditions and results are shown in the table. It can be seen from the table that when the reaction temperature is lower than 100 ° C, the reaction proceeds slowly or not at all (Test 1); when the reaction temperature is 100-110 ° C, a black drug with sufficient activity can be obtained (Test 6). However, the reaction proceeded slowly (190 minutes); at the reaction temperature of 120-140 ° C, the same results as above were obtained, and the reverse time was shortened, and the temperature was increased and the reaction rate was accelerated (tests 4, 7, 10). After the reaction is completed, heating at 170-180 ° C for two hours, the quality of the reaction product is greatly reduced (tests 9, 5, 11, 21, 24), it can be seen that the synthesis temperature is 120-140 ° C, the temperature is too high to produce dimethyl The phenolic dithiophosphoric acid will decompose.
When the pharmaceutical factory produces cresol black medicine, as long as the reaction material is heated to 130 ° C under stirring, the qualified product can be discharged, and the temperature of the product can be lowered to room temperature after a relatively long period of time in the storage. Therefore, it does not need to be heated for 2 hours.
Synthesis and Analysis of Cresol Black Medicine
test
Numbering
Preparation conditions
Xylenol dithiophosphoric acid content (%)
Participate in the weight of the reaction substance
(g)
temperature reflex
(°C)
Reaction time
(Minute)
Heating time after reaction (minutes)
Heating temperature
(°C)
1
6
8
9
3
4
5
7
10
11
Cresol 15.0; CP 2 S 5 5.0
..
..
..
..
..
..
..
..
..
50-60
100-110
100-110
100-110
120
120
120
140
140
140
Reaction does not proceed
190
190
190
105
105
105
55
55
55
-
0
120
120
0
120
120
0
120
120
-
-
120
170-180
-
120
170-180
-
120
170-180
-
53.2
58.8
50.7
48.6
55.4
34.9
54.0
56.7
44.8
20
19
twenty one
Cresol 13.0; CP 2 S 5 5.8
..
..
120
120
120
105
105
105
0
120
120
-
120
170-180
75.3
74.9
29.5
twenty two
twenty three
twenty four
Cresol 13.02; CP 2 S 5 6.0
..
120
120
120
55
55
55
0
120
120
-
120
170-180
70.6
60.6
59.9