CN103803588A - Preparation method of potassium nitrate - Google Patents
Preparation method of potassium nitrate Download PDFInfo
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- CN103803588A CN103803588A CN201310731822.2A CN201310731822A CN103803588A CN 103803588 A CN103803588 A CN 103803588A CN 201310731822 A CN201310731822 A CN 201310731822A CN 103803588 A CN103803588 A CN 103803588A
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Abstract
The invention discloses a preparation method of potassium nitrate. The potassium nitrate is obtained from nitric acid and potassium chloride through ion exchange; the ion exchange is continuous ion exchange by virtue of a plurality of resin columns, and specifically speaking, the feed liquid flows from right to left, while the resin columns rotate clockwise from left to right, and the feed liquid and the resin columns backward act on each other and the process circulates constantly; the plurality of resin columns are orderly divided into an adsorption region and a regeneration region clockwise and orderly. The method is high in safety factor, and the system yield of potassium ions is stabilized above 97%. The concentration of the resolution liquid is about 16.5%, and the content of hydrochloric acid in the adsorption column effluent is about 7%.
Description
Technical field
The present invention relates to chemical field, relate to particularly a kind of preparation method of saltpetre.
Background technology
Saltpetre is a kind of important industrial chemicals, only has at present a small amount of natural Potassium nitrate to exist, and most of saltpetre using is all to rely on chemosynthesis.
In CN92106421.7, disclose a kind of method of utilizing dilute nitric acid production saltpetre, the rare nitric acid that is 35-40 by Repone K and concentration is 70-105 degree in temperature, and negative pressure is that under the condition of 300-400mm mercury column, reaction generates potassium nitrate solution.This method temperature of reaction is high, and potential safety hazard is high.
Ion exchange process for producing potassium nitrate is disclosed in CN96117207.X, with industry or agricultural ammonium nitrate and Repone K be raw material, spent ion exchange resin is exchange carrier, first make it transfer potassium type to by sodium type, and adopt ammonium in following current, potassium in adverse current, to carrying out the exchange of ammonium ion and potassium ion containing ammonium nitrate solution.But ammonium nitrate has explosivity, potential safety hazard is high.
A kind of potassium nitrate preparing technology is disclosed in CN200710062171.7, adopt the nitric acid that Repone K and concentration are 20-40% to mix, under temperature 60-90 degree condition, react, the mixing solutions that generation contains Repone K, rare nitric acid, saltpetre and hydrochloric acid, temperature is fractionation by distillation hydrochloric acid etc. under the condition of 80-95 degree more afterwards.This method temperature is high, and energy consumption is large.
CN201110196387.9 discloses a kind of preparation method of saltpetre, Repone K and nitric acid are dropped in reaction vessel, add water, 45-55 degree dissolves, crystallisation by cooling, then centrifugation makes the mother liquor M1 of saltpetre and containing hydrogen chloride, is dried to obtain saltpetre product, afterwards again with operations such as three octyl tertiary amines and mother liquor M1 extract.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of saltpetre, to solve the above-mentioned problems in the prior art.
Technical scheme provided by the invention is as follows:
A preparation method for saltpetre, adopts nitric acid and Repone K to form through ion-exchange, and described ion-exchange adopts complex root resin column to carry out continuous ionic exchange:
Feed liquid flows from right to left, and resin column is rotated by clockwise direction from left to right, acting in opposition, constantly circulation; The complex root ion exchange resin column of Continuous Moving Bed is divided into adsorption zone and breeding blanket in the direction of the clock successively,
Left side complex root resin column (1-5) of adsorption zone is adsorption column, KCl enters from a feed column (6) on adsorption column right side, after 1 absorption, clean the rinse water of post (7-11) mixes with the right side complex root that comes from this feed column, enter the adsorption column absorption of connecting in left side, wherein, wash water enters from the cleaning post (11) of the rightmost side;
Breeding blanket is divided into resolves district and wash water district, and wherein resolving district's clockwise first (No. 12) is ER post, utilizes product that the water in the pillar before resolving is ejected, and avoids these water to enter desorbed solution, affects desorbed solution concentration; ER post right side is established complex root and is resolved post (13-14), and stripping liquid concentrated nitric acid enters from a desorption column (14) of the rightmost side; Wash water district (No. 15-19) wash water adopts the mode of multicolumn series connection, and wash water enters from the cleaning post (11) of the rightmost side, can improve like this utilization ratio of wash water, reduces wash water consumption, improves desorbed solution concentration;
No. 20 posts are ER post, the rinse water in post are ejected with hydrochloric acid, avoid clear water to enter hydrochloric acid, improve concentration of hydrochloric acid.
Wherein, after ion-exchange, potassium nitrate solution concentrates, and dehydration is dried, and obtains saltpetre.
Wherein, the better content of nitric acid is mass percent 25-40%.Also can adopt the nitric acid of greater concn.But when concentration of nitric acid is greater than 40%, easily there is smog to produce, affect safety.
Wherein, KCE content is mass percent 25-30%.
Wherein, resin column adopts resin cation (R.C.) to carry out ion-exchange.
Wherein, described resin column adopts domestic 001*7 resin cation (R.C.).
Being used for is that concentration is the concentrated nitric acid of 25%-40% by the parsing agent of saltpetre wash-out.
Seen from the above description, the invention provides a kind of preparation method of saltpetre, utilize nitric acid and Repone K to prepare through ion-exchange.When ion-exchange of the present invention, without pyroreaction, safety coefficient is high.Also do not need to adopt extraction agent etc., the potassium nitrate solution of generation can be directly used in processing saltpetre solid.The system yield of potassium ion of the present invention can be stabilized in more than 97%.The concentration of desorbed solution is in 16.5% left and right.In absorption lower column liquid, content of hydrochloric acid is in 7% left and right.
Accompanying drawing explanation
Fig. 1 is preparation method's schematic flow sheet of saltpetre of the present invention.
Embodiment
Embodiment 1
Equipment: the 20 valve port continuous ionic exchange systems that the equipment using provides for SanDa film Science company limited, single-column volume 850ml.Resin filling amount is single-column 650ml, and total consumption is 13L.Charging ram pump used is some.The charging basket used that connects material is some.The resin using is domestic 001*7 resin cation (R.C.).
2, feed liquid: the content using in production is about the KCl solution (concentration is 27.88%) of 278.8g/L
3, nitric acid: concentration is about the concentrated nitric acid (concentration is 35%) of 350g/L
4, water: the evaporation condensed water of production use.
5, resolve agent: concentration 35% concentrated nitric acid
Be below this process flow sheet of testing from friendship continuously, as shown in Figure 1:
1) 20 resin columns of Continuous Moving Bed are divided into Liang Ge district, each district realizes different functions.Wherein first district 1-11 post is adsorption zone; Second 12-20 post is breeding blanket.
2), in Fig. 1, be for No. 1-5 adsorption column.KCl enters from No. 6 posts, after 1 absorption, mixes with the rinse water of 6-11 post below, enters the absorption of connecting of 1--5 post.The unit adsorption rate of resin.
3) be parsing district for No. 12-20.Wherein be for No. 12 ER post, utilize product resolve before pillar in water eject, avoid these water to enter desorbed solution, affect desorbed solution concentration.No. 13-14 for resolving post.No. 15-19 is wash water after resolving, and wash water adopts the mode of multicolumn series connection, can improve like this utilization ratio of wash water, reduces wash water consumption, improves desorbed solution concentration.
4) in this flow process, feed liquid flows from right to left, and resin column rotates from left to right, acting in opposition, and constantly circulation, to realize quantity-produced process.Whole process cycle is 10 hours, 1800 seconds single-column residence time.
Working pressure is low pressure, within the scope of 0.5-2bar.
Embodiment 2-5
Basic identical with embodiment 1, repeat.
The charging of embodiment 1 to 5 and the results are shown in Table 1
Residual acid in desorbed solution (potassium nitrate solution) is detected, and substantially residual acid is in 5% left and right.Than producing, (3% left and right) is slightly high.The concentration of desorbed solution is in 16.5% left and right.In absorption lower column liquid, content of hydrochloric acid is in 7% left and right.
Claims (5)
1. the preparation method of a saltpetre, adopt raw material nitric acid and Repone K to form through ion-exchange, described ion-exchange adopts complex root resin column to carry out continuous ionic exchange: feed liquid flows from right to left, and resin column is rotated by clockwise direction from left to right, acting in opposition, constantly circulation; Complex root ion exchange resin column is divided into adsorption zone and breeding blanket in the direction of the clock successively, wherein,
Left side complex root resin column (1-5) of adsorption zone is adsorption column, KCl enters from a feed column (6) on adsorption column right side, after 1 absorption, clean the rinse water of post (7-11) mixes with the right side complex root that comes from this feed column, enter the adsorption column absorption of connecting in left side, wherein, wash water enters from the cleaning post (11) of the rightmost side;
Breeding blanket is divided into resolves district and wash water district, and wherein resolving district's clockwise first (No. 12) is ER post, utilizes product that the water in the pillar before resolving is ejected, and avoids these water to enter desorbed solution, affects desorbed solution concentration; ER post right side is established complex root and is resolved post (13-14), and stripping liquid concentrated nitric acid enters from a desorption column (14) of the rightmost side; Wash water district (No. 15-19) wash water adopts the mode of multicolumn series connection, and wash water enters from the cleaning post (11) of the rightmost side, can improve like this utilization ratio of wash water, reduces wash water consumption, improves desorbed solution concentration;
An ER post (20) is established on the right side in wash water district, wash water in post is ejected with hydrochloric acid, avoids wash water to reduce concentration of hydrochloric acid;
Raw material nitric acid content used is mass percent 25-40%;
KCE content is mass percent 25-30%;
After ion-exchange, obtain potassium nitrate solution.
2. the preparation method of a kind of saltpetre as claimed in claim 1, is characterized in that, also comprises the steps: that the potassium nitrate solution after ion-exchange concentrates, and dehydration is dried, and obtains solid nitric acid potassium.
3. the preparation method of a kind of saltpetre as claimed in claim 1, is characterized in that: resin column adopts gel type cation resin to carry out ion-exchange.
4. the preparation method of a kind of saltpetre as claimed in claim 3, is characterized in that: described resin column adopts domestic 001*7 Zeo-karb.
5. the preparation method of a kind of saltpetre as claimed in claim 1, is characterized in that: the concentration as the concentrated nitric acid of resolving agent is 25-40%.
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| CN201310731822.2A CN103803588A (en) | 2013-12-26 | 2013-12-26 | Preparation method of potassium nitrate |
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| CN201310731822.2A CN103803588A (en) | 2013-12-26 | 2013-12-26 | Preparation method of potassium nitrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439435A (en) * | 2018-03-24 | 2018-08-24 | 山东天化学股份有限公司 | A kind of method that direct method prepares potassium nitrate |
| CN111410938A (en) * | 2020-01-21 | 2020-07-14 | 山西沃锦新材料股份有限公司 | Binary molten salt and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3645673A (en) * | 1969-12-01 | 1972-02-29 | Dynamit Nobel Ag | Process for the production of potassium nitrate by the ion exchange method |
| US5110578A (en) * | 1989-10-05 | 1992-05-05 | Monomeros Colombo Venezolanos, S.A. (E.M.A.) | Continuous production of potassium nitrate via ion exchange |
| CN102951661A (en) * | 2011-08-19 | 2013-03-06 | 交城县并盛化工有限公司 | Production method of potassium nitrate |
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2013
- 2013-12-26 CN CN201310731822.2A patent/CN103803588A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3645673A (en) * | 1969-12-01 | 1972-02-29 | Dynamit Nobel Ag | Process for the production of potassium nitrate by the ion exchange method |
| US5110578A (en) * | 1989-10-05 | 1992-05-05 | Monomeros Colombo Venezolanos, S.A. (E.M.A.) | Continuous production of potassium nitrate via ion exchange |
| CN102951661A (en) * | 2011-08-19 | 2013-03-06 | 交城县并盛化工有限公司 | Production method of potassium nitrate |
Non-Patent Citations (1)
| Title |
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| 张金辉: "连续离子交换技术在硝酸钾生产中的应用", 《中氮肥》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439435A (en) * | 2018-03-24 | 2018-08-24 | 山东天化学股份有限公司 | A kind of method that direct method prepares potassium nitrate |
| CN111410938A (en) * | 2020-01-21 | 2020-07-14 | 山西沃锦新材料股份有限公司 | Binary molten salt and preparation method thereof |
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Application publication date: 20140521 |