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CN-117660976-B - Pickling corrosion inhibitor and preparation method and application thereof

CN117660976BCN 117660976 BCN117660976 BCN 117660976BCN-117660976-B

Abstract

The invention discloses a preparation method of an acid pickling corrosion inhibitor, which comprises the following steps of obtaining an organic matter A after distillation and drying of brewing bottom water under reduced pressure, extracting, filtering and washing the organic matter A by absolute ethyl alcohol to obtain an organic matter B, adding toluidine, 80% sulfuric acid, potassium iodide and the organic matter B into a reactor, heating and refluxing for 12-18 hours at 135-155 ℃, neutralizing filtrate by adopting a sodium hydroxide solution after acid insoluble matters are removed, then concentrating by reduced pressure distillation, back-extracting by absolute ethyl alcohol, and drying to obtain the acid pickling corrosion inhibitor. The invention can effectively realize the resource utilization of the brewing bottom water, and the prepared pickling corrosion inhibitor has good corrosion inhibition performance.

Inventors

  • ZHENG XINGWEN
  • SU JIAN
  • LI QIJUN
  • LI BEIYAO
  • FAN JINLONG
  • SUN TONG
  • TAN SHUANG

Assignees

  • 宜宾五粮液股份有限公司
  • 四川轻化工大学

Dates

Publication Date
20260505
Application Date
20231215

Claims (10)

  1. 1. The preparation method of the pickling corrosion inhibitor is characterized by comprising the following steps of: (1) Distilling the wine brewing bottom boiler water under reduced pressure and drying to obtain an organic matter A; (2) Extracting the organic matter A obtained in the step (1) by absolute ethyl alcohol, filtering to obtain a liquid phase, and distilling the liquid phase under reduced pressure to obtain an organic matter B; (3) Adding toluidine, 80% sulfuric acid, potassium iodide and the organic matter B obtained in the step (2) into a reactor, heating and refluxing for 12-18 hours at 135-155 ℃, neutralizing filtrate by adopting a sodium hydroxide solution after acid insoluble matters are removed, desalting by using absolute ethyl alcohol, and distilling under reduced pressure until the filtrate is dried, thus obtaining the pickling corrosion inhibitor.
  2. 2. The method for preparing an acid pickling corrosion inhibitor according to claim 1, wherein in the step (1), suspended matters in the brewing bottom water are removed by standing and filtering before reduced pressure distillation.
  3. 3. The method for preparing the pickling corrosion inhibitor according to claim 1, wherein in the step (2), the organic matter A is subjected to ultrasonic extraction for a plurality of times by using absolute ethyl alcohol, and the mass volume ratio of the organic matter A to the absolute ethyl alcohol is1 g:10-30 mL during each extraction.
  4. 4. The method of claim 1, wherein the toluidine in step (3) comprises para-toluidine, meta-toluidine, ortho-toluidine, and homologs thereof.
  5. 5. The method for preparing an acid pickling corrosion inhibitor according to claim 1, wherein in the step (3), the mass ratio of the organic matter B to the toluidine is 1:0.8-1, the addition amount of potassium iodide is 15-25% of the toluidine, and the addition amount of 80% sulfuric acid is 4-6 times of the toluidine.
  6. 6. The method for preparing the pickling corrosion inhibitor according to claim 1, wherein after the reaction in the step (3) is finished, a target product is dissolved by using a sulfuric acid solution, acid insoluble matters are removed by filtration, the product is washed by using the sulfuric acid solution for multiple times until the pumped liquid has no color, then the filtrate is neutralized by using a sodium hydroxide solution, the neutralized filtrate is desalted by using absolute ethyl alcohol, and the pressure is reduced and distilled to dryness, so that the pickling corrosion inhibitor is obtained.
  7. 7. The method for preparing an acid pickling corrosion inhibitor according to claim 6, wherein the concentration of sulfuric acid solution is 1.0-3.0 mol/L, and the concentration of sodium hydroxide solution is 1-6.0 mol/L.
  8. 8. An acid pickling corrosion inhibitor which is characterized by being prepared by adopting the preparation method of the acid pickling corrosion inhibitor disclosed in any one of claims 1-7.
  9. 9. The use of an acid wash corrosion inhibitor according to claim 8 in an acidic solution environment for steel acid wash and oil and gas acid recovery.
  10. 10. The use of an acid pickling corrosion inhibitor according to claim 9, wherein the acidic solution is an aqueous solution of sulfuric acid, hydrochloric acid or nitric acid, the concentration of the acidic solution is 0.1-6 mol/L, and the addition amount of the acid pickling corrosion inhibitor is 0.05-1 g/L.

Description

Pickling corrosion inhibitor and preparation method and application thereof Technical Field The invention belongs to the technical field of resource utilization, and particularly relates to an acid pickling corrosion inhibitor and a preparation method and application thereof. Background According to incomplete statistics, 15-20 tons of brewing wastewater can be produced in the process of producing 1 ton of white spirit in the white spirit production process. The brewing wastewater is an urgent problem of green and high-quality development in the white spirit industry. The brewing bottom water is an important component of brewing wastewater, and is a liquid formed by repeatedly condensing vapor in fermented grains, sinking and gathering the vapor in the bottom of a pot and mixing the vapor with the original water during the process of gelatinizing grains and distilling the fermented grains. As the organic wastewater is used as a steam medium in the distillation link of the fermented grains, organic components are continuously dissolved and leached from the fermented grains in the pot, and the organic wastewater is typical high-concentration organic wastewater. In order to improve the yield of the wine, yellow water is added into the pot to be burned together in the process of baking the wine, so that the ingredients of the bottom pot water are more complex, the treatment difficulty is increased, if the wine is directly discharged, serious environmental pollution is caused, and the resource waste is caused because the organic ingredients in the bottom pot water are not fully utilized. However, the utilization rate of organic resources in the wastewater is low, so that not only is the resource wasted, but also harmful gas is generated and greenhouse gas is discharged due to aerobic and anaerobic treatment. In addition, the resulting sludge further exacerbates the cost of enterprise disposal. The sewage is recycled, and other resources and energy sources are extracted from the sewage, so that the method has important significance in relieving contradiction between supply and demand, reducing water pollution, guaranteeing ecological safety of water, increasing water resource supply and optimizing water supply structure. The white spirit brewing process uses grains as raw materials, and the produced waste water is rich in starch, sugar, organic acid, esters, alcohols and the like, has less harmful substances and has reuse value. Therefore, the treatment mode which can fully recycle resources and simultaneously gives consideration to environmental, social and economic benefits is a main direction of wastewater treatment in the white spirit industry. Corrosion inhibitors, which are agents (chemical substances or compounds) that are effective in alleviating corrosion of metals, are typically added to the environmental medium in which the metal is located to provide protection to the metal. Corrosion inhibitors are widely used in industrial production due to their good performance, low cost and simple operation. The well-known corrosion inhibitor researchers Zheng Gu in China teach that the research of extracting and separating corrosion inhibitor components from natural plants, marine animals and plants and industrial and agricultural wastes and performing chemical modification, and the improvement of the corrosion inhibitor performance is one of the development directions of future corrosion inhibitors. Therefore, if the rich organic matters in the brewing bottom water are used as the corrosion inhibitor for recycling, the method is beneficial to reducing the resource waste, can also reduce the pollution to the environment in the discharge process, and has important practical significance for sustainable development of maintenance and realization of double-carbon economy. Disclosure of Invention Aiming at the defects existing in the prior art, the invention aims to provide an acid pickling corrosion inhibitor, a preparation method and application thereof, the invention can effectively realize the resource utilization of the brewing bottom water, and the prepared pickling corrosion inhibitor has good corrosion inhibition performance. The technical scheme of the invention is realized as follows: The preparation method of the pickling corrosion inhibitor specifically comprises the following steps: (1) Distilling the wine brewing bottom boiler water under reduced pressure and drying to obtain an organic matter A; (2) Extracting, filtering and washing the organic matter A obtained in the step (1) by absolute ethyl alcohol to obtain an organic matter B; (3) Adding toluidine, 80% sulfuric acid, potassium iodide and the organic matter B obtained in the step (2) into a reactor, heating and refluxing for 12-18 hours at 135-155 ℃, neutralizing filtrate by adopting a sodium hydroxide solution after acid insoluble matters are removed, desalting by using absolute ethyl alcohol, and distilling under reduced pressure until the fil