Method of producing petroleum sulfonate by micro reaction system grading sulfonation

A petroleum sulfonate and micro-reaction technology, which is applied in the fields of sulfonate preparation, chemical instruments and methods, organic chemistry, etc., can solve the problem of low ratio of monosulfonate and double sulfonate, insufficient heat transfer capacity of single-stage micro-reaction system, single The problem of high temperature of the outlet material of the micro-reactor is eliminated, and the effect of low temperature, high process efficiency and safety is achieved.

Active Publication Date: 2013-06-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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Problems solved by technology

However, when using this process for production scale-up, in order to promote the uniform distribution of materials in the parallel microchannels of the reactor, the reaction space velocity adopted is 2.5-10 times that of the small test process. At this time, it is found that the heat exchange capacity of the single-stage micro-reaction system Insufficient, resulting in a high temperature of the outlet material of the single-stage microreactor, and a slightly lower content of active matter and the proportion of monosulfonate and disulfonate in the active matter

Method used

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  • Method of producing petroleum sulfonate by micro reaction system grading sulfonation
  • Method of producing petroleum sulfonate by micro reaction system grading sulfonation
  • Method of producing petroleum sulfonate by micro reaction system grading sulfonation

Examples

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Effect test

Embodiment 1

[0027] 25wt.% of sulfonating agent SO 3 About 200kg of the solution is poured into the storage tank 8 for subsequent use; the light distillate oil with a boiling range of 200-450°C and the heavy distillate oil with a boiling range of 260-580°C and dichloroethane solvent are in a mass ratio of 1: 3: The ratio of 4, that is, about 300kg of sulfonated oil with a concentration of 50wt.% is put into the storage tank 6 for subsequent use. The sulfonated oil is continuously delivered to the first-stage microchannel reactor R at a flow rate of 90-95L / h through the metering pump 1 1 In this process, a part of the sulfonating agent is continuously delivered to the first-stage microchannel reactor R through the metering pump 2 at a flow rate of 12.4-32.1L / h 1 In the process, it is mixed with sulfonated oil and undergoes a primary sulfonation reaction, that is, the acid-oil ratio of the primary reaction is 0.085-0.225, and the liquid hourly space velocity in the primary reactor is 35000-...

Embodiment 2

[0032] The reaction process flow is the same as in Example 1. The feed flow rate of the sulfonated oil is fixed, and the total flow rate of the sulfonating agent is changed to 37L / h and 45L / h respectively, that is, the total acid-oil ratio is 0.25 and 0.31, and the liquid sulfur trioxide sulfonating agent is in two stages. Under the distribution ratio of 50:50, 60:40 and 70:30 in the microchannel reactor, two-stage sulfonation was carried out to produce petroleum sulfonic acid.

[0033] Two different total acid-oil ratios are combined with the acid-oil ratio of 0.28 in Example 1, and the product components obtained under the three total ratios include active matter, monosulfonate, inorganic salt and unsulfonated oil and each group The sub-concentration is described by charts 4 and 5.

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Abstract

A method of producing petroleum sulfonate by micro reaction system grading sulfonation includes that a two-stage (or multi-stage) serial micro-channel reaction system is used as a reaction device, each stage micro-channel reaction system is composed of a micro-channel reactor and a micro-channel heat exchanger, and a micro-channel heat exchanger is integrated inside the micro-channel reactor. Petroleum fraction continuously enters from a first stage micro-channel reactor, a liquid sulfur trioxide sulfonating agent respectively enters two stages of the micro-channel reactors according to a certain percentage to react with the petroleum fraction, most reaction heat is removed through the micro-channel heat exchanger integrated inside the micro-channel reactor, two stages of reaction products are respectively and further exchanged heat through the subsequent micro-channel heat exchanger of each stage and heat transferring media all adopts normal temperature industrial circulating water. Compared with single-stage sulfonate, the method of producing the petroleum sulfonate by the micro reaction system grading sulfonation has the advantages of being lower in temperature of reaction of each stage, higher in product active matter content and single and double sulfonates proportion of active matter, capable of improving safety and efficiency of process, and further suitable for pilot scale production and industrialized production.

Description

technical field [0001] The invention relates to a petroleum fraction liquid phase SO in a microreactor 3 The sulfonation method specifically relates to a method for producing petroleum sulfonate by graded sulfonation using micro-reactor technology. Background technique [0002] Oil is a primary strategic resource related to national energy security, but the current oil recovery rate is generally low. Petroleum sulfonate is considered to be the most commercially promising surfactant for tertiary oil recovery due to its wide source of raw materials, large quantity, strong interfacial activity, good compatibility with crude oil, good water solubility, and low cost. Broad distillate SO 3 The production of petroleum sulfonate by liquid phase sulfonation is a rapid and strong exothermic reaction process. The synthetic process of petroleum sulfonate mainly adopts batch tank type and continuous tank type liquid phase sulfonation, and spray film (gas-vapor) sulfonation. Production...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/62C07C303/32B01J19/00
Inventor 陈光文赵玉潮袁权焦凤军李恒强韩梅黄小英刘向东崔继峰付兵张小亮胡元营
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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