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CN112028032A - Regeneration process of sulfuric acid in organic waste sulfuric acid

Publication number

CN112028032A

CN112028032A CN202010934269.2A CN202010934269A CN112028032A CN 112028032 A CN112028032 A CN 112028032A CN 202010934269 A CN202010934269 A CN 202010934269A CN 112028032 A CN112028032 A CN 112028032A

Authority

CN

China

Prior art keywords

sulfuric acid

equipment

acid solution

organic

reaction

Prior art date

2020-09-08

Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)

Pending

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• QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 265
• 230000008929 regeneration Effects 0.000 title claims abstract description 30
• 238000011069 regeneration method Methods 0.000 title claims abstract description 30
• 238000000034 method Methods 0.000 title claims abstract description 22
• 239000010815 organic waste Substances 0.000 title claims abstract description 16
• 238000006243 chemical reaction Methods 0.000 claims abstract description 63
• 239000000463 material Substances 0.000 claims abstract description 36
• 238000004821 distillation Methods 0.000 claims abstract description 34
• 238000004140 cleaning Methods 0.000 claims abstract description 29
• 238000005303 weighing Methods 0.000 claims abstract description 20
• XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
• GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
• 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
• 238000010438 heat treatment Methods 0.000 claims description 30
• 239000002253 acid Substances 0.000 claims description 11
• 239000002699 waste material Substances 0.000 claims description 10
• 238000001035 drying Methods 0.000 claims description 6
• 239000007788 liquid Substances 0.000 claims description 6
• 238000012360 testing method Methods 0.000 claims description 6
• 238000009833 condensation Methods 0.000 claims description 5
• 230000005494 condensation Effects 0.000 claims description 5
• 238000001816 cooling Methods 0.000 claims description 5
• 238000005520 cutting process Methods 0.000 claims description 5
• 238000005086 pumping Methods 0.000 claims description 5
• 230000000087 stabilizing effect Effects 0.000 claims description 5
• 230000001172 regenerating effect Effects 0.000 claims 6
• 238000004519 manufacturing process Methods 0.000 abstract description 4
• 239000012141 concentrate Substances 0.000 abstract description 3
• 238000002360 preparation method Methods 0.000 abstract description 2
• 239000000243 solution Substances 0.000 description 49
• 239000012024 dehydrating agents‎ Substances 0.000 description 3
• 238000010521 absorption reaction Methods 0.000 description 2
• 239000002184 metal Substances 0.000 description 2
• 229910052751 metal Inorganic materials 0.000 description 2
• HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 2
• 238000003723 Smelting Methods 0.000 description 1
• NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
• 230000002378 acidificating effect Effects 0.000 description 1
• 230000004075 alteration Effects 0.000 description 1
• 239000007864 aqueous solution Substances 0.000 description 1
• 230000009286 beneficial effect Effects 0.000 description 1
• 238000009835 boiling Methods 0.000 description 1
• 150000001720 carbohydrates Chemical class 0.000 description 1
• 239000003153 chemical reaction reagent Substances 0.000 description 1
• 239000003795 chemical substances by application Substances 0.000 description 1
• 239000003599 detergent Substances 0.000 description 1
• 229940079593 drug Drugs 0.000 description 1
• 239000003814 drug Substances 0.000 description 1
• 239000000975 dye Substances 0.000 description 1
• 239000002360 explosive Substances 0.000 description 1
• 239000004744 fabric Substances 0.000 description 1
• 239000003337 fertilizer Substances 0.000 description 1
• 239000007789 gas Substances 0.000 description 1
• 239000012535 impurity Substances 0.000 description 1
• 235000013372 meat Nutrition 0.000 description 1
• 150000002739 metals Chemical class 0.000 description 1
• 238000002156 mixing Methods 0.000 description 1
• 238000012986 modification Methods 0.000 description 1
• 230000004048 modification Effects 0.000 description 1
• 239000003208 petroleum Substances 0.000 description 1
• 239000000049 pigment Substances 0.000 description 1
• 239000002994 raw material Substances 0.000 description 1
• 239000007787 solid Substances 0.000 description 1
• 238000003860 storage Methods 0.000 description 1
• 239000000126 substance Substances 0.000 description 1
• 238000006467 substitution reaction Methods 0.000 description 1
• 229910052717 sulfur Inorganic materials 0.000 description 1
• 239000011593 sulfur Substances 0.000 description 1
• 238000003786 synthesis reaction Methods 0.000 description 1
• 239000002023 wood Substances 0.000 description 1

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B17/00—Sulfur; Compounds thereof
  • C01B17/69—Sulfur trioxide; Sulfuric acid
  • C01B17/90—Separation; Purification
  • C01B17/905—Removal of organic impurities

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

The invention discloses a regeneration process of sulfuric acid in organic waste sulfuric acid, which comprises the following steps: A. cleaning sulfuric acid regeneration equipment; B. weighing a proper amount of required reaction materials; C. placing a reaction material inside a reaction vessel; D. carrying out reduced pressure distillation treatment on the reaction material; E. the concentration of generated sulfuric acid is detected; F. the method is simple to operate and easy to implement, can concentrate the organic concentrated sulfuric acid, carbonize organic matters in the organic waste sulfuric acid and generate nitric acid solution, reduces the manufacturing cost of the concentrated sulfuric acid, and separates out water in the organic waste sulfuric acid through reduced pressure distillation, so that the sulfuric acid solution is concentrated, the nitric acid solution is obtained, and the method has enough economic applicability and can be widely applied to preparation of the concentrated sulfuric acid and the nitric acid solution.

Technical Field

The invention relates to the technical field of preparation and production of concentrated sulfuric acid, in particular to a regeneration process of sulfuric acid in organic waste sulfuric acid.

Background

Sulfuric acid is the most important oxyacid of sulfur and is highly acidic. The anhydrous sulfuric acid is colorless oily liquid, is crystallized at 10.36 ℃, is usually prepared by various aqueous solutions with different concentrations by a tower method and a contact method, the former is crude dilute sulfuric acid, and the mass fraction is about 75 percent generally; the latter can obtain 98.3% mass percentage of concentrated sulfuric acid, boiling point is 338 ℃, relative density is 1.84, sulfuric acid is the most active binary inorganic strong acid, can react with most metals, high concentration sulfuric acid has strong water absorption, can be used as dehydrating agent, and can be used for dehydrating agent, carbonized wood, paper, cotton-linen fabric, biological skin and meat and other carbohydrate-containing substances, when mixed with water, a large amount of heat energy can be released, and the sulfuric acid has strong corrosivity and oxidizability, so the sulfuric acid needs to be used carefully. The organic waste sulfuric acid is an important industrial raw material, can be used for manufacturing fertilizers, medicines, explosives, pigments, detergents, storage batteries and the like, is widely applied to industries of purifying petroleum, metal smelting, dyes and the like, is commonly used as a chemical reagent, can be used as a dehydrating agent and a sulfonating agent in organic synthesis, can be obtained only by blending solid sulfuric acid in a strange way, is difficult to be directly distilled because the concentrated sulfuric acid has strong water absorption, can be dried by soda lime to obtain the concentrated sulfuric acid, but can generate corrosive gases such as NO and NO2 in the process of preparing the concentrated sulfuric acid by drying the soda lime, so that how to economically and practically distill the organic waste sulfuric acid becomes a difficult problem which needs to be solved at present. .

Disclosure of Invention

The invention aims to provide a sulfuric acid regeneration process which is simple to operate and easy to implement, can concentrate organic concentrated sulfuric acid, carbonize organic matters in organic waste sulfuric acid and generate nitric acid solution, and reduces the production cost of the concentrated sulfuric acid.

In order to achieve the purpose, the invention provides the following technical scheme: a specific operation method of a sulfuric acid regeneration process in organic waste sulfuric acid comprises the following steps:

A. cleaning sulfuric acid regeneration equipment;

B. weighing a proper amount of required reaction materials;

C. placing a reaction material inside a reaction vessel;

D. carrying out reduced pressure distillation treatment on the reaction material;

E. the concentration of generated sulfuric acid is detected;

F. cleaning sulfuric acid regeneration equipment and airing.

Preferably, the clean sulfuric acid regeneration plant is finished according to step a:

a. cleaning and debugging a waste acid distillation kettle and condensing equipment;

b. testing the pressure reduction equipment and the heating equipment to confirm that the equipment is intact and can be normally used;

c. and checking the connection condition of the condensing equipment to confirm that the connection is tight and reliable.

Preferably, the appropriate amount of the desired reaction material is weighed according to step B:

a. weighing a proper amount of organic sulfuric acid solution;

b. and weighing a proper amount of pure water according to the weighed organic sulfuric acid solution.

Preferably, the reaction material is placed inside the reaction vessel according to step C:

a. slowly injecting organic sulfuric acid solution into the reaction heating kettle;

b. adding weighed pure water into the condensation container;

c. sufficient condensed liquid is added to the exterior of the condensing vessel.

Preferably, the reaction material is treated by distillation under reduced pressure according to step D:

a. heating organic sulfuric acid solution in the distillation kettle to 200 ℃;

b. adjusting the internal pressure of the reaction equipment to 0.9 times of atmospheric pressure by using vacuum pumping equipment;

c. heating the organic sulfuric acid solution to 280 deg.c and the pressure inside the reactor to 0.85 times the atmospheric pressure.

Preferably, the concentration of the generated sulfuric acid is checked according to step E:

a. heating the organic sulfuric acid solution to 300 ℃, and stabilizing the internal pressure of the reaction equipment by 0.8 times of atmospheric pressure;

b. cutting off the connection with the condensing equipment to stop heating the sulfuric acid solution;

c. and (3) when the concentration of the sulfuric acid solution is tested by cooling the sulfuric acid solution and meets the preset standard, taking out the sulfuric acid solution, and continuing carrying out reduced pressure distillation when the concentration does not meet the preset standard.

Preferably, the sulfuric acid regeneration plant is cleaned and dried according to step F:

a. cleaning a waste acid distillation kettle, nitric acid solution condensing equipment and accessory equipment thereof;

b. wiping or drying the cleaned equipment;

c. the dried cleaning equipment is placed regularly for standby.

Compared with the prior art, the invention has the beneficial effects that:

(1) the step A arrangement clean sulfuric acid regeneration equipment provided by the invention can prevent foreign impurities from influencing the purity of the sulfuric acid generated by the reaction.

(2) B, weighing a proper amount of required reaction materials to ensure that the concentration of the concentrated sulfuric acid is in direct proportion to the concentration of the generated nitric acid solution

(3) Step C, placing the reaction material in the reaction container, and carrying out reduced pressure distillation treatment on the reaction material in the step D, so that the sulfuric acid can be effectively purified in a low pressure distillation mode.

(4) Step E tests to generate sulfuric acid concentration, so that the concentrated sulfuric acid concentration can meet the preset requirement, and step F cleans sulfuric acid regeneration equipment and dries the sulfuric acid regeneration equipment, so that the used equipment is clean and tidy, and the next use is prevented from being influenced.

Drawings

FIG. 1 is a schematic view of the operation flow structure of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The first embodiment is as follows:

as shown in fig. 1, the specific operation method comprises the following steps:

A. cleaning sulfuric acid regeneration equipment;

B. weighing a proper amount of required reaction materials;

C. placing a reaction material inside a reaction vessel;

D. carrying out reduced pressure distillation treatment on the reaction material;

E. the concentration of generated sulfuric acid is detected;

F. cleaning sulfuric acid regeneration equipment and airing.

The clean sulfuric acid regeneration equipment is finished according to step a:

a. cleaning and debugging a waste acid distillation kettle and condensing equipment;

b. testing the pressure reduction equipment and the heating equipment to confirm that the equipment is intact and can be normally used;

c. and checking the connection condition of the condensing equipment to confirm that the connection is tight and reliable.

Weighing a proper amount of required reaction materials according to the step B:

a. weighing a proper amount of organic sulfuric acid solution;

b. and weighing a proper amount of pure water according to the weighed organic sulfuric acid solution.

Placing the reaction material inside the reaction vessel according to step C:

a. slowly injecting organic sulfuric acid solution into the reaction heating kettle;

b. adding weighed pure water into the condensation container;

c. sufficient condensed liquid is added to the exterior of the condensing vessel.

Carrying out reduced pressure distillation treatment on the reaction material according to the step D:

a. heating organic sulfuric acid solution in the distillation kettle to 200 ℃;

b. adjusting the internal pressure of the reaction equipment to 0.9 times of atmospheric pressure by using vacuum pumping equipment;

c. heating the organic sulfuric acid solution to 280 deg.c and the pressure inside the reactor to 0.85 times the atmospheric pressure.

Checking the concentration of generated sulfuric acid according to step E:

a. heating the organic sulfuric acid solution to 300 ℃, and stabilizing the internal pressure of the reaction equipment by 0.8 times of atmospheric pressure;

b. cutting off the connection with the condensing equipment to stop heating the sulfuric acid solution;

c. and (3) when the concentration of the sulfuric acid solution is tested by cooling the sulfuric acid solution and meets the preset standard, taking out the sulfuric acid solution, and continuing carrying out reduced pressure distillation when the concentration does not meet the preset standard.

Cleaning and airing sulfuric acid regeneration equipment according to the step F:

a. cleaning a waste acid distillation kettle, nitric acid solution condensing equipment and accessory equipment thereof;

b. wiping or drying the cleaned equipment;

c. the dried cleaning equipment is placed regularly for standby.

Example two:

as shown in fig. 1, the specific operation method comprises the following steps:

A. cleaning sulfuric acid regeneration equipment;

B. weighing a proper amount of required reaction materials;

C. placing a reaction material inside a reaction vessel;

D. carrying out reduced pressure distillation treatment on the reaction material;

E. the concentration of generated sulfuric acid is detected;

F. cleaning sulfuric acid regeneration equipment and airing.

The clean sulfuric acid regeneration equipment is finished according to step a:

a. cleaning and debugging a waste acid distillation kettle and condensing equipment;

b. testing the pressure reduction equipment and the heating equipment to confirm that the equipment is intact and can be normally used;

c. and checking the connection condition of the condensing equipment to confirm that the connection is tight and reliable.

Weighing a proper amount of required reaction materials according to the step B:

a. weighing a proper amount of organic sulfuric acid solution;

b. and weighing a proper amount of pure water according to the weighed organic sulfuric acid solution.

Placing the reaction material inside the reaction vessel according to step C:

a. slowly injecting organic sulfuric acid solution into the reaction heating kettle;

b. adding weighed pure water into the condensation container;

c. sufficient condensed liquid is added to the exterior of the condensing vessel.

Carrying out reduced pressure distillation treatment on the reaction material according to the step D:

a. heating organic sulfuric acid solution in the distillation kettle to 100 ℃;

b. adjusting the internal pressure of the reaction equipment to 0.9 times of atmospheric pressure by using vacuum pumping equipment;

c. heating the organic sulfuric acid solution to 150 deg.c and the pressure inside the reactor to 0.85 times atmospheric pressure.

Checking the concentration of generated sulfuric acid according to step E:

a. heating the organic sulfuric acid solution to 200 ℃, and stabilizing the internal pressure of the reaction equipment by 0.8 times of atmospheric pressure;

b. cutting off the connection with the condensing equipment to stop heating the sulfuric acid solution;

c. and (3) when the concentration of the sulfuric acid solution is tested by cooling the sulfuric acid solution and meets the preset standard, taking out the sulfuric acid solution, and continuing carrying out reduced pressure distillation when the concentration does not meet the preset standard.

Cleaning and airing sulfuric acid regeneration equipment according to the step F:

a. cleaning a waste acid distillation kettle, nitric acid solution condensing equipment and accessory equipment thereof;

b. wiping or drying the cleaned equipment;

c. the dried cleaning equipment is placed regularly for standby.

Example three:

as shown in fig. 1, the specific operation method comprises the following steps:

A. cleaning sulfuric acid regeneration equipment;

B. weighing a proper amount of required reaction materials;

C. placing a reaction material inside a reaction vessel;

D. carrying out reduced pressure distillation treatment on the reaction material;

E. the concentration of generated sulfuric acid is detected;

F. cleaning sulfuric acid regeneration equipment and airing.

The clean sulfuric acid regeneration equipment is finished according to step a:

a. cleaning and debugging a waste acid distillation kettle and condensing equipment;

b. testing the pressure reduction equipment and the heating equipment to confirm that the equipment is intact and can be normally used;

c. and checking the connection condition of the condensing equipment to confirm that the connection is tight and reliable.

Weighing a proper amount of required reaction materials according to the step B:

a. weighing a proper amount of organic sulfuric acid solution;

b. and weighing a proper amount of pure water according to the weighed organic sulfuric acid solution.

Placing the reaction material inside the reaction vessel according to step C:

a. slowly injecting organic sulfuric acid solution into the reaction heating kettle;

b. adding weighed pure water into the condensation container;

c. sufficient condensed liquid is added to the exterior of the condensing vessel.

Carrying out reduced pressure distillation treatment on the reaction material according to the step D:

a. heating organic sulfuric acid solution in the distillation kettle to 50 ℃;

b. adjusting the internal pressure of the reaction equipment to 0.9 times of atmospheric pressure by using vacuum pumping equipment;

c. heating the organic sulfuric acid solution to 100 deg.c and the pressure inside the reactor to 0.85 times atmospheric pressure.

Checking the concentration of generated sulfuric acid according to step E:

a. heating the organic sulfuric acid solution at 150 deg.c and stabilizing the pressure inside the reactor to 0.8 times the atmospheric pressure;

b. cutting off the connection with the condensing equipment to stop heating the sulfuric acid solution;

c. and (3) when the concentration of the sulfuric acid solution is tested by cooling the sulfuric acid solution and meets the preset standard, taking out the sulfuric acid solution, and continuing carrying out reduced pressure distillation when the concentration does not meet the preset standard.

Cleaning and airing sulfuric acid regeneration equipment according to the step F:

a. cleaning a waste acid distillation kettle, nitric acid solution condensing equipment and accessory equipment thereof;

b. wiping or drying the cleaned equipment;

c. the dried cleaning equipment is placed regularly for standby.

In conclusion, the embodiment I distills and concentrates the organic sulfuric acid to obtain higher sulfuric acid concentration, and has better economical and practical properties.

The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention, so long as the technical solutions can be realized on the basis of the above embodiments without creative efforts, which should be considered to fall within the protection scope of the patent of the present invention.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

1. A process for regenerating sulfuric acid in organic waste sulfuric acid comprises the following steps:

A. cleaning sulfuric acid regeneration equipment;

B. weighing a proper amount of required reaction materials;

C. placing a reaction material inside a reaction vessel;

D. carrying out reduced pressure distillation treatment on the reaction material;

E. the concentration of generated sulfuric acid is detected;

F. cleaning sulfuric acid regeneration equipment and airing.

2. The process for regenerating sulfuric acid from organic waste sulfuric acid according to claim 1, wherein the clean sulfuric acid regeneration equipment is arranged according to step a:

a. cleaning and debugging a waste acid distillation kettle and condensing equipment;

b. testing the pressure reduction equipment and the heating equipment to confirm that the equipment is intact and can be normally used;

c. and checking the connection condition of the condensing equipment to confirm that the connection is tight and reliable.

3. The process for regenerating sulfuric acid from organic waste sulfuric acid as claimed in claim 1, wherein a proper amount of the required reaction materials are weighed according to step B:

a. weighing a proper amount of organic sulfuric acid solution;

b. and weighing a proper amount of pure water according to the weighed organic sulfuric acid solution.

4. The process for regenerating sulfuric acid from organic waste sulfuric acid as claimed in claim 1, wherein the reaction material is placed inside the reaction vessel according to step C:

a. slowly injecting organic sulfuric acid solution into the reaction heating kettle;

b. adding weighed pure water into the condensation container;

c. sufficient condensed liquid is added to the exterior of the condensing vessel.

5. The process of claim 1, wherein the reduced pressure distillation is performed according to step D to treat the reaction material:

a. heating organic sulfuric acid solution in the distillation kettle to 200 ℃;

b. adjusting the internal pressure of the reaction equipment to 0.9 times of atmospheric pressure by using vacuum pumping equipment;

c. heating the organic sulfuric acid solution to 280 deg.c and the pressure inside the reactor to 0.85 times the atmospheric pressure.

6. The process for regenerating sulfuric acid from organic waste sulfuric acid according to claim 1, wherein the concentration of generated sulfuric acid is determined according to step E:

a. heating the organic sulfuric acid solution to 300 ℃, and stabilizing the internal pressure of the reaction equipment by 0.8 times of atmospheric pressure;

b. cutting off the connection with the condensing equipment to stop heating the sulfuric acid solution;

c. and (3) when the concentration of the sulfuric acid solution is tested by cooling the sulfuric acid solution and meets the preset standard, taking out the sulfuric acid solution, and continuing carrying out reduced pressure distillation when the concentration does not meet the preset standard.

7. The process for regenerating sulfuric acid from organic waste sulfuric acid according to claim 1, wherein the sulfuric acid regeneration equipment is cleaned and dried according to step F:

a. cleaning a waste acid distillation kettle, nitric acid solution condensing equipment and accessory equipment thereof;

b. wiping or drying the cleaned equipment;

c. the dried cleaning equipment is placed regularly for standby.

• 2020
  • 2020-09-08 CN CN202010934269.2A patent/CN112028032A/en active Pending

Application publication date: 20201204

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