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Process for producing ammonium dibutyl dithiophosphate

A production process and technology of butylammonium black medicine, applied in the field of production technology of butylammonium black medicine, can solve the problems of high energy consumption, large number of condensers, environmental protection pressure, etc. in the production process, so as to reduce production and maintenance costs and production process. Simple and effective in increasing production capacity

Inactive Publication Date: 2018-11-27
YANTAI HUMON CHEM AUX CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The traditional process of butylammonium black medicine is drying method, the disadvantages of traditional production process: 1. Because the traditional production process will produce a small amount of black medicine residue in the process of producing butylammonium black medicine, resulting in the intermediate product dibutyl dithiophosphoric acid ( Butylic acid black drug) content is relatively low, so the synthesized dibutyl dithiophosphoric acid (butylic acid black drug) must be put into a settling tank to stand still, and the settled dibutyl dithiophosphoric acid (butyl Acid black medicine) and dilute it with water to a certain concentration before the neutralization reaction can be carried out. The black medicine residue in the settling tank is easy to pollute the environment and cause pressure on environmental protection
2. In the traditional production process, dibutyl dithiophosphoric acid (butyric acid black drug) needs to be diluted with water before neutralization, so the butyl ammonium black drug solution must be dried with a scraper dryer to obtain solid butyl ammonium black medicine; this production process consumes a lot of energy, the output per unit time is low, the process is relatively complicated, and the number of auxiliary equipment such as vacuum pumps and condensers is large, and the maintenance cost is also high.
3. The volume of the traditional scraper dryer is small, the output per unit time is low, and the cost is high

Method used

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  • Process for producing ammonium dibutyl dithiophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: Prepare n-butanol 400g, phosphorus pentasulfide 300g, add 0.2g pyridine as catalyst, reaction temperature 90 ℃, react for 2.5 hours, the reaction time is extended appropriately to improve intermediate product dibutyldithiophosphoric acid (butyrate black conversion rate of medicine); since most of the black medicine residues are unreacted coarse grains of phosphorus pentasulfide and black medicine acid, and there will be a small amount of double black medicine generated by side reactions, adding a catalyst can inhibit the occurrence of side reactions; Reaction time, to improve the transformation rate of intermediate product black medicine acid, thereby reduce the amount of black medicine residue;

[0017] Add the generated dibutyl dithiophosphoric acid (butylic acid black drug) into the kneader, feed frozen brine into the jacket of the kneader to cool down, and then feed ammonia gas by weighing (500g of butylic acid black drug is added to 40 -50g ammonia ga...

Embodiment 2

[0018] Example 2: Prepare 400 g of isobutanol, 300 g of phosphorus pentasulfide, add 0.2 g of pyridine as a catalyst, and react at a reaction temperature of 90° C. for 2.5 hours;

[0019] Add the generated dibutyl dithiophosphoric acid (butylic acid black drug) into the kneader, feed frozen brine into the jacket of the kneader to cool down, and then feed ammonia gas by weighing (500g of butylic acid black drug is added to 40 -50g ammonia gas), control the reaction temperature at 75°C for 3 hours, control the pH=8-9 after the reaction, and directly obtain the finished product of butyl ammonium black medicine.

[0020] In the new production process, the intermediate product dibutyl dithiophosphoric acid (butyric acid black drug) is weighed and metered into the kneader, the reactor is started, and then ammonia gas is metered in for reaction. Since the reactor uses a kneader, The material reacts and mixes more fully in the kneader, so the butyric acid black medicine does not need ...

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Abstract

The invention provides a process for producing ammonium dibutyl dithiophosphate. The process comprises the following steps: (1) taking butanol and phosphorus pentasulfide according to a weight ratio of 4:3, adding pyridine as a catalyst, wherein the addition amount of the pyridine is 1 / 2000 of the weight of the butanol, controlling the reaction temperature to be 90 DEG C, reacting for 2.5 hours, and synthesizing dibutyl dithiophosphate; and (2) adding the dibutyl dithiophosphate produced in the step (1) into a kneading machine, introducing frozen brine into a jacket of the kneading machine forcooling, and slowly introducing ammonia gas, wherein the introduction amount of the ammonia gas is 4-5 / 50 of the weight of the ammonium dibutyl dithiophosphate, controlling the reaction temperature to be 70-75 DEG C, reacting for 3 hours, reaching the endpoint when the pH value of the reaction solution is 8-9, and directly obtaining the finished ammonium dibutyl dithiophosphate. According to theprocess disclosed by the invention, the production process of the ammonium dibutyl dithiophosphate is simple, the operation is easy, the capacity of the ammonium dibutyl dithiophosphate is greatly improved, any ammonium dibutyl dithiophosphate residue is not produced in the whole process procedure, environmental protection is realized, and the product quality is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a production process of ammonium butyl ammonium black medicine. Background technique [0002] The traditional process of butylammonium black medicine is drying method, the disadvantages of traditional production process: 1. Because the traditional production process will produce a small amount of black medicine residue in the process of producing butylammonium black medicine, resulting in the intermediate product dibutyl dithiophosphoric acid ( Butylic acid black drug) content is relatively low, so the synthesized dibutyl dithiophosphoric acid (butylic acid black drug) must be put into a settling tank to stand still, and the settled dibutyl dithiophosphoric acid (butyl Acid black medicine) and dilute it with water to a certain concentration to carry out the neutralization reaction. The black medicine residue in the settling tank is easy to pollute the environment and ca...

Claims

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Application Information

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IPC IPC(8): C07F9/17
CPCC07F9/17
Inventor 曲华东于新阳徐庆华
Owner YANTAI HUMON CHEM AUX CO LTD
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