CN104108690A - Equipment and process for preparing electronic grade nitric acid having a concentration of 68% from industrial grade nitric acid having a concentration of 98% - Google Patents

Equipment and process for preparing electronic grade nitric acid having a concentration of 68% from industrial grade nitric acid having a concentration of 98% Download PDF

Info

Publication number
CN104108690A
CN104108690A CN201410256682.2A CN201410256682A CN104108690A CN 104108690 A CN104108690 A CN 104108690A CN 201410256682 A CN201410256682 A CN 201410256682A CN 104108690 A CN104108690 A CN 104108690A
Authority
CN
China
Prior art keywords
nitric acid
header tank
tower
rectifying tower
raw material
Prior art date
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.)
Granted
Application number
CN201410256682.2A
Other languages
Chinese (zh)
Other versions
CN104108690B (en
Inventor
刘鸣
赵云翰
刘利娟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd
Original Assignee
SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd filed Critical SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd
Priority to CN201410256682.2A priority Critical patent/CN104108690B/en
Publication of CN104108690A publication Critical patent/CN104108690A/en
Application granted granted Critical
Publication of CN104108690B publication Critical patent/CN104108690B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Manufacture And Refinement Of Metals (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Equipment for preparing electronic grade nitric acid having a concentration of 68% from industrial grade nitric acid having a concentration of 98% is disclosed. The equipment comprises a rectifying tower provided with heating coils made of metal tantalum. The rectifying tower is filled with a glass raschig ring filling material. The diameter of the rectifying tower is 180-250 mm and the height of the rectifying tower is 5-10 m. A process for preparing the electronic grade nitric acid having a concentration of 68% from the industrial grade nitric acid having a concentration of 98% is also disclosed. The diameter of the rectifying tower is set to be 180-250 mm, the height of the rectifying tower is set to be 5-10 m, the reflux ratio is controlled to be 1:2-1:5, the heating coils in the rectifying tower are made of the metal tantalum, and the rectifying tower is filled with the glass raschig ring filling material. According to the equipment and the process, a finished high-purity product of the electronic grade nitric acid can be prepared by one time of distillation, thus saving resources and reducing pollution.

Description

By 98% technical grade nitric acid, made equipment and the technique of electronic-grade 68% nitric acid
Technical field
The present invention relates to a kind of equipment and technique that is made electronic-grade 68% nitric acid by 98% technical grade nitric acid.
Background technology
Nitric acid is one of common inorganic acid, in semi-conductor, flat pannel display, photovoltaic industry etching, has very large effect.Common electronic grade high-purity 68% nitric acid process of preparing generally selects SILVER REAGENT 70% nitric acid as raw material, then adopts distil process to remove metal ion, residue, particle etc. to reach the applicable specification of semi-conductor.It is directly 98% nitric acid that but general industryization is produced product, SILVER REAGENT 70% nitric acid is by diluting, distill and blow white cooling resulting product by 98% nitric acid, and as raw material again rectifying by repeat consumption steam, water circulates, pressurized air etc., due to needs second distillation, waste resource, increased production cost.In Chinese invention patent, the patent No. is 201110041529.4 method for producing electronic-grade nitric acid, the chemically pure reagent level nitric acid material of concentration 70% left and right is provided, the 70% SILVER REAGENT nitric acid that known its rectification process adopts, also by technical grade 98% nitric acid dilution rectifying, formed, therefore cost is higher, uses starting material for SILVER REAGENT nitric acid simultaneously, and this technique does not have technical grade nitric acid is purified and become the ability of Nitric acid of highly purity as seen.
Need 98% technical grade nitric acid could be made to electronic-grade 68% nitric acid by second distillation at present, and the each distillation of nitric acid all can decomposite part NO 2gas, this part gas cannot be dissolved in nitric acid again, must from nitric acid, remove by the method for gas displacement, and this part gas is directly disposed in atmosphere or the mode absorbing by water is dissolved in the water, all can cause the pollution of N, affect environment, repeatedly distillation will repeatedly produce pollution; In addition, after distillation condensation, all can produce noncondensable gas, this part gas is mainly the mixed gas of nitric acid and oxynitride, and nitric acid distills condensation at every turn all can produce this part gas, contaminate environment.
Why 98% nitric acid directly not being diluted to rectifying is at present 68% high pure nitric acid, because type of heating is indirect heating, heating coil is glass or tetrafluoro or lining fluorine or other plastic materials, poor thermal conductivity, need to consume mass energy, and plain metal can not tolerate the nitric acid of 98% concentration, cause that to add the rectifying tower height of thermal material limited, cannot utilize higher stage number to carry out rectifying.
In sum, at present, the technique of electronic grade high-purity 68% nitric acid has that cost is high, the wasting of resources, easily cause the shortcoming of topsoil.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of single flash just to reach final Nitric acid of highly purity product, both saved the resources such as steam, recirculated water, pressurized air, can reduce again because of distillation, blow the white NO causing 2discharge, reduce atmosphere, water pollution by technical grade nitric acid, make equipment and the technique of electronic-grade nitric acid.
For achieving the above object, technical scheme of the present invention is as follows: a kind of equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid, comprise rectifying tower, in described rectifying tower, be provided with heating coil, the material of described heating coil is metal tantalum, in described rectifying tower, be filled with glass Raschig ring filler, the tower diameter of described rectifying tower is 180-250mm, and tower height is 5-10m.
Preferably, comprise PLC, nitric acid header tank, pure water header tank, raw material header tank, described nitric acid header tank, pure water header tank is connected with raw material header tank respectively, described raw material header tank is connected with the bottom of reboiler and the bottom of rectifying tower, the top of described reboiler is connected with the middle part of rectifying tower, the outlet of described nitric acid header tank is provided with nitric acid under meter, the outlet of described pure water header tank is provided with pure water under meter, between described raw material header tank and reboiler, be provided with feed rate meter, on described reboiler, be provided with steam pressure regulator and tower reactor thermometer, described PLC respectively with nitric acid under meter, pure water under meter, feed rate meter, steam pressure regulator and tower reactor thermometer connect.
Preferably, comprise pipe connecting, described raw material header tank is provided with at least two, the outlet of described nitric acid header tank, the outlet of pure water header tank all has outlet pipe, the entrance of each raw material header tank has inlet tube, described two outlet pipes are communicated with one end of pipe connecting, the other end of described pipe connecting is communicated with two inlet tubes, on described two outlet pipes and two root entry pipes, be respectively arranged with the first magnetic valve, described pure water under meter is arranged on the outlet pipe of pure water header tank, described nitric acid under meter is arranged on the outlet pipe of nitric acid header tank, described in each, in raw material header tank, be provided with raw material liquidometer, described each raw material liquidometer and each the first magnetic valve connect with PLC respectively.
Preferably, described distillation tower top is rotated and is provided with tower top, and described equipment also comprises driving cylinder, and described driving cylinder and tower top are rotationally connected, and described driving cylinder connects with PLC.
Preferably, also comprise primary condenser, blow White Tower, after-condenser and finished pot, the top of described rectifying tower, primary condenser, blow White Tower, after-condenser and finished pot and connect successively.
Preferably, described finished pot is provided with at least two, described at least two finished pots are connected with after-condenser respectively, between described each finished pot and after-condenser, be provided with the second magnetic valve, described in each, in finished pot, be provided with automatic tank gauge, described each second magnetic valve, each automatic tank gauge connect with PLC respectively.
A kind of technique that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid, described technology utilization is to making the equipment of electronic-grade nitric acid by technical grade nitric acid in power 1-power 6, step 1, the tower diameter of rectifying tower is set to 180-250mm, tower height is set to 5-10m, control reflux ratio is 1:2-1:5, and the heating coil material in rectifying tower is set to metal tantalum, is filled with glass Raschig ring filler in rectifying tower; Step 2, PLC opens and closes by controlling described nitric acid header tank, pure water header tank the first magnetic valve respectively and between raw material header tank, then controls in nitric acid and the pure water incoming stock header tank 3 of volume ratio with 45:34-46:31; Step 3, part material enters rectifying tower through reboiler, remainder directly enters rectifying tower, it is 150-200L/h to the inlet amount in reboiler that PLC controls raw material header tank by control feed rate meter, and the pressure that PLC controls in reboiler is 0.2-0.3Mpa, 98% nitric acid enters in rectifying tower, and heating coil is heated to 120-125 ℃ by the temperature in rectifying tower, and the glass Raschig ring filler in rectifying tower is removed metal ion, residue, granule foreign to 98% nitric acid; Step 4, the work in-process that obtain by rectifying from discharge at rectifying tower top, then enter successively primary condenser, blow White Tower, after-condenser, finally enter finished pot.
Preferably, raw material header tank in step 2 has at least two, and raw material liquidometer shows the liquid level in raw material header tank, and PLC receives the liquid level that raw material liquidometer shows, PLC controls the first magnetic valve and opens and closes, and nitric acid and pure water are entered in the raw material header tank that liquid level is lower.
Preferably, finished pot in step 4 has at least two, automatic tank gauge shows the liquid level in finished pot, PLC receives after the liquid level numerical value of automatic tank gauge demonstration, PLC controls the second magnetic valve and opens and closes, and the 68% nitric acid finished product of the electronic-grade after after-condenser is entered in the finished pot that liquid level is lower.
Adopt the beneficial effect of the technical program to be:
One, the material of the heating coil in rectifying tower is metal tantalum, in rectifying tower, be filled with glass Raschig ring filler, the tower diameter of rectifying tower is 180-250mm, tower height is 5-10m, reflux ratio is 1:2-1:5, adopt metal tantalum as the material of heating coil, can tolerate the nitric acid of 98% concentration, and good heat conductivity, can be directly to 98% the rare heating of nitric acid, and can effectively remove metal ion by glass Raschig ring filler, residue, the impurity such as particle are partly led the applicable specification of technique body to reach, single flash, technical grade 98% nitric acid can be made to electronic grade high-purity 68% nitric acid, reduce distillation number of times, reduced energy consumption, reduced NO 2exhaust emission, improved quality,
They are two years old, PLC is set, PLC connects with nitric acid under meter, pure water under meter, raw material liquidometer, each first magnetic valve, feed rate meter, steam pressure regulator, tower reactor thermometer, the second magnetic valve, automatic tank gauge respectively, and whole-course automation is controlled, and controls comparatively accurate and quick.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in embodiment of the present invention technology, to the accompanying drawing of required use in embodiment technical description be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of the present embodiment.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Consult shown in Fig. 1, a kind of equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid, comprise rectifying tower 5, in rectifying tower 5, be provided with heating coil 19, the material of heating coil 19 is metal tantalum, in rectifying tower 5, be filled with glass Raschig ring filler, the tower diameter of rectifying tower 5 is 180-250mm, and tower height is 5-10m.The tower diameter of the rectifying tower 5 in the present embodiment is 230mm, and tower height is 7m.
Distillation is the unit operation in Principles of Chemical Engineering, it is completely separated with low-boiling point material that all high boiling materials can fall in theory, in the present embodiment, adopting material is direct technical grade 98% nitric acid of heating coil 19 of metal tantalum, can tolerate the nitric acid of 98% concentration, and good heat conductivity, can be directly to 98% nitric acid heating, effectively solved poor thermal conductivity, need to consume mass energy, and cause that to add the rectifying tower height of thermal material limited, cannot utilize higher stage number to carry out the problem of rectifying, nitric acid fully can be heated by more theoretical plate number, thereby reach more good separating effect, and can effectively remove metal ion by glass Raschig ring filler, residue, the impurity such as particle are partly led the applicable specification of technique body to reach, final technical grade product just can be reached by single flash to semi-conductor electricity sub level chemical reagent.The ratio of the tower height of rectifying tower 5 and tower diameter, for designing the parameter that chemical industry rectifying device must be definite, can be determined discharging speed the most suitable on guaranteed quality basis by adjusting reflux ratio simultaneously.Adopt single flash 98% technical grade nitric acid can be made to electronic-grade 68% nitric acid, reduced NO 2gas is directly disposed in atmosphere or the mode absorbing by water is dissolved in the water, the pollution then causing, and minimizing distillation number of times just can reach and fall oligosaprobic effect; Meanwhile, also reduce the generation of the noncondensable gas producing after distillation condensation, further reduced pollution.
The equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid comprises PLC, nitric acid header tank 1, pure water header tank 2, raw material header tank 3, nitric acid header tank 1, pure water header tank 2 is connected with raw material header tank 3 respectively, raw material header tank 3 is connected with the bottom of reboiler 4 and the bottom of rectifying tower 5, the top of reboiler 4 is connected with the middle part of rectifying tower 5, the outlet of nitric acid header tank 1 is provided with nitric acid under meter 11, the outlet of pure water header tank 2 is provided with pure water under meter 10, between raw material header tank 3 and reboiler 4, be provided with feed rate meter 14, on reboiler 4, be provided with steam pressure regulator 16 and tower reactor thermometer 15, PLC respectively with nitric acid under meter 11, pure water under meter 10, feed rate meter 14, steam pressure regulator 16 and tower reactor thermometer 15 connect.By PLC respectively with nitric acid under meter 11, pure water under meter 10, feed rate meter 14, steam pressure regulator 16 and tower reactor thermometer 15 connect, by PLC, control nitric acid under meter 11, pure water under meter 10 is controlled nitric acid then, the volume ratio of the incoming stock header tank 3 of pure water, by PLC, controlling feed rate meter 14 then controls 98% the nitric acid that enters reboiler 4 and enters the flow in reboiler 4, by tower reactor thermometer 15, the temperature of steam pressure regulator 16 feedbacks and the numerical value of vapor pressure, PLC is adjusted to desirable value by the temperature in reboiler 4 and vapor pressure, automatization is controlled, comparatively accurate.
This equipment comprises pipe connecting 22, raw material header tank 3 is provided with at least two, the outlet of nitric acid header tank 1, the outlet of pure water header tank 2 all has outlet pipe 21, the entrance of each raw material header tank 3 has inlet tube 23, two outlet pipes 21 are communicated with one end of pipe connecting 22, the other end of pipe connecting 22 is communicated with two inlet tubes 23, on two outlet pipes 21 and two root entry pipes 23, be respectively arranged with the first magnetic valve 12, pure water under meter 10 is arranged on the outlet pipe 21 of pure water header tank 2, nitric acid under meter 11 is arranged on the outlet pipe 21 of nitric acid header tank 1, in each raw material header tank 3, be provided with raw material liquidometer 13, each raw material liquidometer 13 and each the first magnetic valve 12 connect with PLC respectively.Automatization is controlled, PLC receives the liquid level numerical value that the raw material liquidometer 13 in raw material header tank 3 shows, PLC controls the first magnetic valve 12 and opens and closes, and nitric acid and pure water are entered in the raw material header tank 3 that liquid level is lower with certain volume ratio, and efficiency, precision are high.
Distillation tower 5 tops are rotated and are provided with tower top 17, and equipment also comprises driving cylinder 20, drive cylinder 20 and tower top 17 to be rotationally connected, and drive cylinder to connect with PLC.Tower top 17 temperature when tower top 17 evaporates in order to control, control still-process according to this temperature, and the open and close of tower top 17 are controlled and driven cylinder 20 to realize by PLC.
Same as the prior art, this equipment also comprises primary condenser 6, blows White Tower 7, after-condenser 8 and finished pot 9, the top of rectifying tower 5, primary condenser 6, blows White Tower 7, after-condenser 8 and finished pot 9 and connects successively.
Finished pot 9 is provided with at least two, at least two finished pots 9 are connected with after-condenser 8 respectively, between each finished pot 9 and after-condenser 8, be provided with the second magnetic valve 18, in each finished pot 9, be provided with automatic tank gauge 20, the second magnetic valves 18, each automatic tank gauge 20 connects with PLC respectively.Automatic tank gauge 20 is in order to show the liquid level that makes finished product in finished pot 9 corresponding thereto, PLC receives after the liquid level being fed back by automatic tank gauge 20, PLC controls two the second magnetic valves 18 again and opens and closes, electronic-grade 68% nitric acid finished product is entered in the finished pot 9 that liquid level is lower, automatization is controlled, and comparatively accurate, finished pot 9 is provided with at least two, the 68% nitric acid finished product can unremitting storage making, has improved efficiency.
A kind of technique that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid, this technology utilization is to the above-mentioned equipment that is made electronic-grade nitric acid by technical grade nitric acid, step 1, the tower diameter of rectifying tower 5 is set to 180-250mm, tower height is set to 5-10m, control reflux ratio is 1:2-1:5, and heating coil 19 materials in rectifying tower 5 are set to metal tantalum, are filled with glass Raschig ring filler in rectifying tower 5; The tower diameter of the rectifying tower 5 in the present embodiment is 230mm, and tower height is 7m, and reflux ratio is 1:3; Step 2, PLC opens and closes by controlling nitric acid header tank 1, pure water header tank 2 the first magnetic valve 12 respectively and between raw material header tank 3, then control in nitric acid and the pure water incoming stock header tank 3 of volume ratio with 45:34-46:31, the volume ratio in the present embodiment is 45:34; Step 3, part material enters rectifying tower 5 through reboiler 4, remainder directly enters rectifying tower 5, it is 150-200L/h to the inlet amount in reboiler 4 that PLC controls raw material header tank 3 by control feed rate meter 14, inlet amount in the present embodiment is 200L/h, and the pressure that PLC controls in reboiler 4 is 0.2-0.3Mpa, 98% nitric acid enters in rectifying tower 5, heating coil 19 is heated to 120-125 ℃ by the temperature in rectifying tower 5, and the glass Raschig ring filler in rectifying tower 5 is removed metal ion, residue, granule foreign to 98% nitric acid; Step 4, the work in-process that obtain by distillation from discharge at rectifying tower 5 tops, then enter successively primary condenser 6, blow White Tower 7, after-condenser 8, finally enter finished pot 9.
Wherein, raw material header tank 3 in step 2 has at least two, the liquid level that raw material liquidometer 13 shows in raw material header tank 3, PLC receives the liquid level that raw material liquidometer 13 shows, PLC controls the first magnetic valve 12 and opens and closes, and nitric acid and pure water are entered in the raw material header tank 3 that liquid level is lower.
Finished pot 9 in step 4 has at least two, the liquid level that automatic tank gauge 20 shows in finished pot 9, PLC receives after the liquid level numerical value of automatic tank gauge 20 demonstrations, PLC controls the second magnetic valve 18 and opens and closes, and the 68% nitric acid finished product of the electronic-grade after after-condenser 8 is entered in the finished pot 9 that liquid level is lower.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (9)

1. an equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid, comprise rectifying tower, in described rectifying tower, be provided with heating coil, it is characterized in that: the material of described heating coil is metal tantalum, in described rectifying tower, be filled with glass Raschig ring filler, the tower diameter of described rectifying tower is 180-250mm, and tower height is 5-10m.
2. the equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 1, it is characterized in that: comprise PLC, nitric acid header tank, pure water header tank, raw material header tank, described nitric acid header tank, pure water header tank is connected with raw material header tank respectively, described raw material header tank is connected with the bottom of reboiler and the bottom of rectifying tower, the top of described reboiler is connected with the middle part of rectifying tower, the outlet of described nitric acid header tank is provided with nitric acid under meter, the outlet of described pure water header tank is provided with pure water under meter, between described raw material header tank and reboiler, be provided with feed rate meter, on described reboiler, be provided with steam pressure regulator and tower reactor thermometer, described PLC respectively with nitric acid under meter, pure water under meter, feed rate meter, steam pressure regulator and tower reactor thermometer connect.
3. the equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 2, it is characterized in that: comprise pipe connecting, described raw material header tank is provided with at least two, the outlet of described nitric acid header tank, the outlet of pure water header tank all has outlet pipe, the entrance of each raw material header tank has inlet tube, described two outlet pipes are communicated with one end of pipe connecting, the other end of described pipe connecting is communicated with two inlet tubes, on described two outlet pipes and two root entry pipes, be respectively arranged with the first magnetic valve, described pure water under meter is arranged on the outlet pipe of pure water header tank, described nitric acid under meter is arranged on the outlet pipe of nitric acid header tank, described in each, in raw material header tank, be provided with raw material liquidometer, described each raw material liquidometer and each the first magnetic valve connect with PLC respectively.
4. the equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 2, it is characterized in that: described distillation tower top is rotated and is provided with tower top, described equipment also comprises driving cylinder, and described driving cylinder and tower top are rotationally connected, and described driving cylinder connects with PLC.
5. the equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 2, it is characterized in that: also comprise primary condenser, blow White Tower, after-condenser and finished pot, the top of described rectifying tower, primary condenser, blow White Tower, after-condenser and finished pot and connect successively.
6. the equipment that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 5, it is characterized in that: described finished pot is provided with at least two, described at least two finished pots are connected with after-condenser respectively, between described each finished pot and after-condenser, be provided with the second magnetic valve, described in each, in finished pot, be provided with automatic tank gauge, described each second magnetic valve, each automatic tank gauge connect with PLC respectively.
7. by technical grade 98% nitric acid, made a technique for electronic-grade 68% nitric acid, described technology utilization, to making the equipment of electronic-grade nitric acid by technical grade nitric acid in power 1-power 6, is characterized in that:
Step 1, the tower diameter of rectifying tower is set to 180-250mm, and tower height is set to 5-10m, and control reflux ratio is 1:2-1:5, and the heating coil material in rectifying tower is set to metal tantalum, is filled with glass Raschig ring filler in rectifying tower;
Step 2, PLC opens and closes by controlling described nitric acid header tank, pure water header tank the first magnetic valve respectively and between raw material header tank, then controls in nitric acid and the pure water incoming stock header tank 3 of volume ratio with 45:34-46:31;
Step 3, part material enters rectifying tower through reboiler, remainder directly enters rectifying tower, it is 150-200L/h to the inlet amount in reboiler that PLC controls raw material header tank by control feed rate meter, and the pressure that PLC controls in reboiler is 0.2-0.3Mpa, 98% nitric acid enters in rectifying tower, and heating coil is heated to 120-125 ℃ by the temperature in rectifying tower, and the glass Raschig ring filler in rectifying tower is removed metal ion, residue, granule foreign to 98% nitric acid;
Step 4, the work in-process that obtain by rectifying from discharge at rectifying tower top, then enter successively primary condenser, blow White Tower, after-condenser, finally enter finished pot.
8. the technique that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 7, it is characterized in that: the raw material header tank in step 2 has at least two, raw material liquidometer shows the liquid level in raw material header tank, PLC receives the liquid level that raw material liquidometer shows, PLC controls the first magnetic valve and opens and closes, and nitric acid and pure water are entered in the raw material header tank that liquid level is lower.
9. the technique that is made electronic-grade 68% nitric acid by technical grade 98% nitric acid according to claim 7, it is characterized in that: the finished pot in step 4 has at least two, automatic tank gauge shows the liquid level in finished pot, PLC receives after the liquid level numerical value of automatic tank gauge demonstration, PLC controls the second magnetic valve and opens and closes, and the 68% nitric acid finished product of the electronic-grade after after-condenser is entered in the finished pot that liquid level is lower.
CN201410256682.2A 2014-06-11 2014-06-11 Equipment and the technique of electron level 68% nitric acid is prepared by 98% technical grade nitric acid Active CN104108690B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410256682.2A CN104108690B (en) 2014-06-11 2014-06-11 Equipment and the technique of electron level 68% nitric acid is prepared by 98% technical grade nitric acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410256682.2A CN104108690B (en) 2014-06-11 2014-06-11 Equipment and the technique of electron level 68% nitric acid is prepared by 98% technical grade nitric acid

Publications (2)

Publication Number Publication Date
CN104108690A true CN104108690A (en) 2014-10-22
CN104108690B CN104108690B (en) 2016-06-15

Family

ID=51705709

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410256682.2A Active CN104108690B (en) 2014-06-11 2014-06-11 Equipment and the technique of electron level 68% nitric acid is prepared by 98% technical grade nitric acid

Country Status (1)

Country Link
CN (1) CN104108690B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111994885A (en) * 2020-08-25 2020-11-27 福建天甫电子材料有限公司 Preparation device and preparation process for electronic-grade nitric acid
CN112279225A (en) * 2020-11-16 2021-01-29 河南骏化发展股份有限公司 Production system and process for co-production of industrial-grade nitric acid and electronic-grade nitric acid
CN113493192A (en) * 2021-08-09 2021-10-12 联仕(昆山)化学材料有限公司 Production process of electronic-grade nitric acid
CN114538393A (en) * 2022-03-04 2022-05-27 福建富轩科技有限公司 Nitric acid purification automatic control system
CN115028147A (en) * 2022-06-30 2022-09-09 江苏淮河化工有限公司 Process for continuously preparing electronic-grade nitric acid by rectification and stripping integrated method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139864A (en) * 2011-02-21 2011-08-03 上海正帆科技有限公司 Method for producing electronic-grade nitric acid
CN202020932U (en) * 2011-04-11 2011-11-02 江阴市润玛电子材料有限公司 Rectification device for ultra-pure nitric acid
CN203187406U (en) * 2013-03-26 2013-09-11 江阴润玛电子材料股份有限公司 Energy-saving nitric acid purifying device
CN103359698A (en) * 2013-07-30 2013-10-23 江阴江化微电子材料股份有限公司 Purification system for industrial production of electronic grade nitric acid

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139864A (en) * 2011-02-21 2011-08-03 上海正帆科技有限公司 Method for producing electronic-grade nitric acid
CN202020932U (en) * 2011-04-11 2011-11-02 江阴市润玛电子材料有限公司 Rectification device for ultra-pure nitric acid
CN203187406U (en) * 2013-03-26 2013-09-11 江阴润玛电子材料股份有限公司 Energy-saving nitric acid purifying device
CN103359698A (en) * 2013-07-30 2013-10-23 江阴江化微电子材料股份有限公司 Purification system for industrial production of electronic grade nitric acid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111994885A (en) * 2020-08-25 2020-11-27 福建天甫电子材料有限公司 Preparation device and preparation process for electronic-grade nitric acid
CN111994885B (en) * 2020-08-25 2021-12-24 福建天甫电子材料有限公司 Preparation device and preparation process for electronic-grade nitric acid
CN112279225A (en) * 2020-11-16 2021-01-29 河南骏化发展股份有限公司 Production system and process for co-production of industrial-grade nitric acid and electronic-grade nitric acid
CN113493192A (en) * 2021-08-09 2021-10-12 联仕(昆山)化学材料有限公司 Production process of electronic-grade nitric acid
CN113493192B (en) * 2021-08-09 2022-07-29 联仕(昆山)化学材料有限公司 Production process of electronic-grade nitric acid
WO2023015603A1 (en) * 2021-08-09 2023-02-16 联仕(昆山)化学材料有限公司 Electronic-grade nitric acid production process
CN114538393A (en) * 2022-03-04 2022-05-27 福建富轩科技有限公司 Nitric acid purification automatic control system
CN115028147A (en) * 2022-06-30 2022-09-09 江苏淮河化工有限公司 Process for continuously preparing electronic-grade nitric acid by rectification and stripping integrated method

Also Published As

Publication number Publication date
CN104108690B (en) 2016-06-15

Similar Documents

Publication Publication Date Title
CN104108690A (en) Equipment and process for preparing electronic grade nitric acid having a concentration of 68% from industrial grade nitric acid having a concentration of 98%
CN103466629B (en) A kind of polycrystalline silicon reducing furnace temperature control energy-saving system and technique
CN103449443A (en) Heat energy recovery system and technology of water system of polycrystalline silicon reducing furnace
CN203852856U (en) Seven-effect and three-section evaporation indirect-condensation evaporator set for concentrated sodium aluminate solution
CN206304378U (en) The energy-conservation MVR evaporators that a kind of vapor recompression is utilized
CN203006955U (en) 72-cobar polycrystalline silicon reduction furnace
CN203852855U (en) Six-efficiency three-segment evaporation indirect condensation evaporator group for concentrated sodium aluminate solution
CN206572485U (en) A kind of coal-ethylene glycol steam condensate heat recycling system
CN103394204B (en) Acid bath multi-effect liquid film evaporating process and device
CN103523761A (en) Continuous nitric acid discoloring device and method thereof
CN204395477U (en) A kind of economic benefits and social benefits crystallizing evaporator
CN109019725A (en) A kind of energy conservation water vaporization tower
CN102249849A (en) Device for producing anhydrous alcohol
CN204325200U (en) The optimization device of alcohol tower and recovery tower in methylamine distillation system
CN204854127U (en) Circulating water system in salt manufacturing production technology
CN104477955B (en) Live steam condensed water cooling in a kind of alumina producing and heat recovery method
CN206843114U (en) One kind energy-conservation water vaporization tower
CN104194636A (en) Colophony production equipment
CN213698866U (en) Circulating type ethylene glycol distillation system
CN205917031U (en) Phosphoric acid refrigeration cycle water vacuum device
CN104803828A (en) Device and method for improving 1,4-butanediol yield
CN204745714U (en) Rectifying column temperature regulation and control device
CN214232825U (en) Methanol pre-tower fine-remaining device
CN205174897U (en) Steam condensate hydrothermal can and for water conservancy device
CN205170709U (en) A device for improving 1, 4 - butanediol yield

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant