Bio-based alkyl thiophosphoric acid or derivative thereof and preparation method and application of bio-based alkyl thiophosphoric acid or derivative thereof
An alkylthiophosphoric acid, a bio-based technology, applied in the field of machinery or material science, can solve the problems of petrochemical resource loss, complex production process, and poor practical applicability, and achieve the effect of renewable raw materials and environmental friendliness
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Embodiment 1
[0061] Embodiment 1 (comparative example)
[0062] In this example, dodecylphenol is used to synthesize sulfuric acid and its derivatives. Dodecylphenol is alkylated by phenol and tetrapropylene (isododecene) under the catalysis of cation exchange resin or activated clay. be made of.
[0063] Synthesis of thiophosphoric acid: 22.23gP 2 S 5 Put 10.0g of 150N base oil into a reaction bottle, heat to 70°C and stir to disperse, then add 110.1g of dodecylphenol dropwise into the mixture, and control the rate of addition so that the temperature does not exceed 105°C due to the exothermic reaction. After the dropwise addition was completed and the temperature was maintained at 105°C for 1 hour, the temperature was raised to 125°C. After maintaining for 1 hour, purging with nitrogen, the hydrogen sulfide gas in the system was tested negative with lead acetate test paper, and the reaction was completed. After filtration, the phosphoric acid content in the product was 89%, P was 4.3...
Embodiment 2
[0066] In this example, biogenic phenol was used to synthesize phosphoric acid and its derivatives.
[0067] Synthesis of thiophosphoric acid: 22.23gP 2 S 5 Put 10.0g of 150N base oil into a reaction bottle, heat to 70°C and stir to disperse, then add 63.0g of thymol dropwise to the mixture, and control the rate of addition so that the temperature does not exceed 105°C due to the exothermic reaction. After the dropwise addition was completed and the temperature was maintained at 105°C for 1 hour, the temperature was raised to 125°C. After maintaining for 1 hour, purging with nitrogen, the hydrogen sulfide gas in the system was tested negative with lead acetate test paper, and the reaction was completed. After filtration, the phosphoric acid content in the product was 85.7%, P was 6.7%, and S was 13.8%.
[0068] Neutralization reaction: Add 9.13g of ZnO to 30g of 150N base oil and 30g of thymolyl sulfuric acid, stir to disperse. Heat to 45-50°C, add dropwise the remaining 7...
Embodiment 3-10
[0070] Embodiment 3-10 adopts monohydric alcohol of biological origin and its mixture to synthesize phosphoric acid and its derivatives. The synthesis steps are the same as in Example 1 or 2. The specific phosphoric acid synthesis temperature and time vary according to different raw materials. The specific feed ratio is the same as The results are shown in Table 1 and Table 2.
[0071] Table 1
[0072] Example
Types of bio-based alcohols
P 2 S 5 (g)
Alcohol 1 (g)
Alcohol 2 (g)
150N(g)
P%
S%
Example 3
22.2
31.1
-
10.0
80.8%
10.3%
21.4%
Example 4
2-butanol
22.2
31.1
-
10.0
80.8%
10.3%
21.4%
Example 5
n-octanol
22.2
54.7
-
10.0
84.9%
7.4%
15.4%
[0073] Example 6
1-pentanol
22.2
37.0
-
10.0
82.1%
9.4%
19.5%
Example 7
sec-butanol, 2-pentanol
22.2
13.8
20....
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