CN111111793A - Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate - Google Patents
Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate Download PDFInfo
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- CN111111793A CN111111793A CN202010041131.XA CN202010041131A CN111111793A CN 111111793 A CN111111793 A CN 111111793A CN 202010041131 A CN202010041131 A CN 202010041131A CN 111111793 A CN111111793 A CN 111111793A
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- way valve
- ion exchange
- hydroxylamine
- exchange column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/14—Hydroxylamine; Salts thereof
- C01B21/1409—Preparation
Abstract
The invention discloses an ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate, wherein the ion exchange device comprises an ion exchange column and a three-way valve, the bottom end of the ion exchange column is provided with a third three-way valve, and the top end of the ion exchange column is provided with an IV three-way valve and a V three-way valve; one end of the third three-way valve is connected with a vent pipeline, and the other end of the third three-way valve is connected with the second three-way valve; one end of the IV three-way valve is connected with a vent pipeline, and the other end of the IV three-way valve is connected with a discharge pipe; one end of the fifth three-way valve is connected with an emptying pipeline, and the other end of the fifth three-way valve is connected with the fifth three-way valve; one end of the first three-way valve is connected with a feeding pipe, the other end of the first three-way valve is connected with the second three-way valve, and the other end of the second three-way valve is connected with a discharging pipe; the I three-way valve and the II three-way valve are arranged at the same height, and the IV three-way valve and the V three-way valve are arranged at the same height and are higher than the I three-way valve and the II three-way valve. The device can improve the utilization efficiency of resin and reduce the consumption of raw materials; the phenomenon of empty tower or tower overflow is avoided; the pollution of residual materials in the pipeline to the subsequent operation is solved.
Description
Technical Field
The invention relates to a preparation process of hydroxylamine nitrate or hydroxylamine perchlorate, in particular to a process and a device for preparing hydroxylamine nitrate or hydroxylamine perchlorate by adopting cation exchange resin.
Background
Hydroxylamine salts are compounds formed from hydroxylamine and an acid, and mainly include hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine nitrate, hydroxylamine perchlorate and the like. The synthesis method of the hydroxylamine salt is divided according to a raw material route, and the synthesis method mainly comprises two types, wherein one type is directly synthesized from the beginning by adopting methods such as catalytic reduction and the like, and the other type is prepared from the existing other types of water-soluble hydroxylamine salt by methods such as double decomposition reaction and the like.
Hydroxylamine hydrochloride and hydroxylamine sulfate are stable in properties, and are industrially produced on a large scale by a nitrogen monoxide reduction method, a sodium nitrite synthesis method, a nitromethane method, a disulfonic acid ammonium salt hydrolysis method, a ketoxime hydrolysis method, a newly developed hydrogen peroxide oxidation method, and the like.
The hydroxylamine nitrate and the hydroxylamine perchlorate have high energy and relatively poor stability, and the technology for directly synthesizing the hydroxylamine nitrate has high difficulty and high equipment investment; compared with hydroxylamine nitrate, hydroxylamine perchlorate has stronger oxidation to anions and is more difficult to directly synthesize. For this purpose, hydroxylamine nitrate or perchlorate is generally obtained by conversion from hydroxylamine hydrochloride or hydroxylamine sulfate.
The method for switching different kinds of hydroxylamine salts includes a double decomposition method and an ion exchange method. Yangxin method [ preparation and performance analysis of hydroxylamine perchlorate, bulletin, 1987, 2], and Chamber [ research and development of hydroxylamine perchlorate for synthesizing propellant by ion exchange method, propulsion technology, 1999, V (20): and 4, Zhang Mengming [ synthesis and characterization of hydroxylamine perchlorate, bulletin of explosives and powders, 2013, V (36): 4; factors affecting ion exchange of exchange resin with hydroxylamine in HAP synthesis, 2014, V (12): 1] et al report experimental research on synthesizing hydroxylamine perchlorate by an ion exchange method, documents all adopt a top-down concurrent feeding process, and examine the influence of resin grade, feeding coefficient, feeding rate and the like on resin exchange capacity and hydroxylamine perchlorate yield in detail, without relating to the influence of the ion exchange process on test operation and test results.
It was found that the following problems exist in the preparation of hydroxylamine nitrate or hydroxylamine perchlorate from hydroxylamine hydrochloride (sulphate) using the existing ion exchange process: (1) the repeated exchange phenomenon caused by the exchange zone is obvious in the alternate process of adsorption-acid washing and removing, a part of resin bed layers in the ion exchange column can not be effectively utilized, the raw material consumption is large, and the production capacity is low; (2) because the composition, concentration and density of effluent liquid in the ion exchange process are constantly changed, the material inlet and outlet rates of the ion exchange column are difficult to keep balance all the time, an operator is required to monitor and carefully adjust the material inlet and outlet rates constantly, air resistance can occur slightly carelessly to cause empty columns or overflow columns, the operation procedure is complicated, and the stability is poor. Therefore, practical production and preparation of hydroxylamine nitrate or hydroxylamine perchlorate are difficult and costly.
Disclosure of Invention
The first purpose of the invention is to provide an ion exchange device, which can improve the utilization efficiency of resin and reduce the consumption of raw materials; the phenomenon of empty tower or tower overflow is avoided; the pollution of residual materials in the pipeline to the subsequent operation is solved.
The second purpose of the invention is to provide the application of the ion exchange device in the ion exchange process for preparing hydroxylamine nitrate or hydroxylamine perchlorate.
In order to realize the first invention purpose, the technical scheme of the invention is as follows: an ion exchange device comprises an ion exchange column and a three-way valve, and is characterized in that a third three-way valve h is arranged at the bottom end of the ion exchange column, and an IV three-way valve e and a V three-way valve f are arranged at the top end of the ion exchange column; one end of the third three-way valve h is connected with a vent pipeline, and the other end of the third three-way valve h is connected with the second three-way valve d; one end of the IV three-way valve e is connected with a vent pipeline, and the other end of the IV three-way valve e is connected with a discharge pipe b; one end of the V-th three-way valve f is connected with a vent pipeline, and the other end of the V-th three-way valve f is connected with the I-th three-way valve c; one end of the first three-way valve c is connected with a feeding pipe a, the other end of the first three-way valve c is connected with a second three-way valve d, and the other end of the second three-way valve d is connected with a discharging pipe b; the I-th three-way valve c and the II-th three-way valve d are installed at the same height, and the IV-th three-way valve e and the V-th three-way valve f are installed at the same height and are higher than the I-th three-way valve c and the II-th three-way valve d.
The function of the I three-way valve c is to switch the feeding of the raw material hydroxylamine salt and the elution acid; the function of the II three-way valve d is to switch the charging of the hydroxylamine salt and the discharging of the eluent; the third three-way valve h is used for switching the feeding of the hydroxylamine salt as the raw material, the discharging of the eluent and the column emptying; the IV three-way valve e is used for switching the discharging and emptying of the adsorption residual liquid; the function of the V-th three-way valve f is to switch the elution acid feed and vent. And a pipeline between the II-th three-way valve d and the III-th three-way valve h is used as a feed pipe of the hydroxylamine salt raw material and a discharge pipe of the eluent.
In order to realize the second invention purpose, the technical scheme of the invention is as follows: an ion exchange process for preparing hydroxylamine nitrate or hydroxylamine perchlorate by adopting cation exchange resin comprises the following steps:
(1) adsorption: and switching the valve, adsorbing the measured hydroxylamine salt solution from the lower part to the upper part of the ion exchange column through the I three-way valve c, the II three-way valve d and the III three-way valve h, and flowing out the adsorption residual liquid from the discharge pipe through the IV three-way valve e. The hydroxylamine salt solution refers to an aqueous solution of hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine oxalate, hydroxylamine phosphate, or the like.
(2) Washing with water: and (3) washing the ion exchange column with pure water according to the feeding mode of the step (1) until the hydroxylamine salt serving as the raw material cannot be detected in the washing liquid.
(3) And (3) elution: and switching the valve, adding metered nitric acid aqueous solution or perchloric acid aqueous solution into the ion exchange column from top to bottom through the I three-way valve c and the V three-way valve f for elution, enabling eluent to flow out of the bottom of the ion exchange column through the III three-way valve h, turning over along a pipeline to pass through the II three-way valve d upwards, and discharging and collecting the eluent through a discharging pipe.
(4) Washing with water: and (4) washing the ion exchange column with pure water according to the feeding mode of the step (3) until the pH value of the effluent liquid is detected to be neutral.
And (4) effluent liquid of the steps (3) and (4) is diluted hydroxylamine nitrate or hydroxylamine perchlorate solution, and the product can be obtained after further concentration and crystallization.
Suitable cation exchange resins include 732 type (001X 7), 001X 4 type, 001X 8 type, Dowex-50, Amberlite IR-120, Lewatit-100, etc., which have been previously subjected to acid activation treatment.
Compared with the prior art, the ion exchange device and the process have the following beneficial effects: by adopting a countercurrent feeding mode, the volume of a resin bed layer which cannot be effectively utilized due to repeated exchange in the ion exchange column is reduced, the utilization efficiency of the resin is improved to over 49 percent from the original 25.9 percent, and the consumption of raw materials is reduced by over 50 percent; the discharge pipeline at the bottom of the column is turned over upwards instead of directly flowing downwards and then flows out, and the liquid level controls the balance of the material inlet and outlet speeds of the ion exchange column, so that empty or overflow of the column is avoided, the operation is simple and convenient, and the stability is good; part of the feeding pipes of the raw material hydroxylamine salt during adsorption and the discharging pipes of the eluent during elution are combined for use, and material switching is performed through the three-way valve, so that dead angles of pipelines and material residues are reduced, and the problems that the material residues pollute subsequent operation during countercurrent feeding and the like are solved.
Drawings
FIG. 1 is a schematic view of an ion exchange unit according to the present invention.
Wherein, a feeding pipe b, a discharging pipe c, an I three-way valve d, an II three-way valve e, an IV three-way valve f, a V three-way valve g, a cation exchange column h, a III three-way valve
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that these examples are for illustrative purposes only and are not intended to limit the present invention. Any modification of the present invention within the scope not departing from the gist of the invention is within the scope of the invention as claimed.
As shown in fig. 1, an ion exchange device comprises an ion exchange column and a three-way valve, and is characterized in that a third three-way valve h is installed at the bottom end of the ion exchange column, and an IV three-way valve e and a V three-way valve f are installed at the top end of the ion exchange column; one end of the third three-way valve h is connected with a vent pipeline, and the other end of the third three-way valve h is connected with the second three-way valve d; one end of the IV three-way valve e is connected with a vent pipeline, and the other end of the IV three-way valve e is connected with a discharge pipe b; one end of the V-th three-way valve f is connected with a vent pipeline, and the other end of the V-th three-way valve f is connected with the I-th three-way valve c; one end of the first three-way valve c is connected with a feeding pipe a, the other end of the first three-way valve c is connected with a second three-way valve d, and the other end of the second three-way valve d is connected with a discharging pipe b; the I-th three-way valve c and the II-th three-way valve d are installed at the same height, and the IV-th three-way valve e and the V-th three-way valve f are installed at the same height and are higher than the I-th three-way valve c and the II-th three-way valve d. The ion exchange column was loaded with a 007X 7 type cation exchange resin which had been previously activated.
Example 1
Switching a valve, adding 682mL of 10% hydroxylamine sulfate aqueous solution into an ion exchange column with the diameter of phi 3.5 multiplied by 40cm (the resin filling amount is 370mL) from bottom to top at the flow rate of 11-12 mL/min, and enabling the adsorption residual liquid to flow out from the top of the ion exchange column through an IV three-way valve e; after adsorption, adding pure water into the ion exchange column for washing in the manner until sulfate ions can not be detected in the washing liquid; switching the valve again, adjusting the flow rate to 5-6 mL/min, adding 152mL of nitric acid aqueous solution into the ion exchange column from top to bottom, enabling the eluent to flow out of the bottom of the column through the third three-way valve h, upwards pass through the fourth three-way valve e, then discharging and collecting the eluent through the discharge pipe b, and detecting the pH value of the eluent, wherein the pH value of the eluent is preferably not lower than 3.0; and finally, washing with pure water until the pH value of the water washing liquid is neutral. And (3) receiving the eluent and the water washing liquid with the pH value of more than 3.0, and detecting that the eluent and the water washing liquid contain 23g of hydroxylamine nitrate, wherein the resin utilization efficiency is 49.6%.
Example 2
322mL of a 10% aqueous solution of hydroxylamine sulfate was added to a 3.5X 40cm diameter ion exchange column, and the procedure was as in example 1. And detecting the eluent and the water washing liquid with the pH value of more than 3.0, wherein the eluent and the water washing liquid contain 22.8g of hydroxylamine nitrate, the utilization efficiency of the resin is 49.2 percent, and the dosage of the hydroxylamine sulfate serving as a raw material is reduced by 52.7 percent.
Example 3
The procedure of example 1 was repeated except that 276mL of a 10% aqueous solution of hydroxylamine hydrochloride was charged into an ion exchange column having a diameter of 3.5X 40 cm. And detecting the eluent and the water washing liquid with the pH value of more than 3.0, wherein the eluent and the water washing liquid contain 22.9g of hydroxylamine nitrate, and the utilization efficiency of the resin is 49.3 percent. The consumption of the hydroxylamine hydrochloride raw material is reduced by 52.7 percent.
Example 4
322mL of a 10% aqueous solution of hydroxylamine sulfate was added to a Φ 3.5X 40cm ion exchange column, and adsorption and water washing were performed as in example 1. After washing, switching a valve, adjusting the flow rate to 7-8 mL/min, adding 315mL perchloric acid aqueous solution into the ion exchange column from top to bottom, enabling eluent to flow out of the bottom of the column through a third three-way valve h, upwards pass through an IV three-way valve e, then discharging and collecting the eluent in a discharge pipe b, and preferably detecting the pH value of the eluent to be not lower than 3.0; and finally washing with pure water until the pH value of the water washing liquid is neutral. And (3) receiving the eluent and the water washing liquid with the pH value of more than 3.0, and detecting that 42.1g of hydroxylamine perchlorate is contained in the eluent and the resin utilization efficiency is 65.3%.
Example 5
5157mL of a 10% hydroxylamine sulfate aqueous solution was added to an ion exchange column having a diameter of 8.0X 100cm (resin loading of 4300mL) from the bottom up at a flow rate of 60 to 65mL/min, and adsorption and washing were performed as in example 1. And after washing, switching a valve, adjusting the flow rate to 50-55 mL/min, adding 6650mL of nitric acid aqueous solution into the ion exchange column from top to bottom for elution, and then washing with pure water until the pH value of the washing solution is detected to be neutral. And collecting the eluent and the water washing liquid, and detecting that the eluent contains 360g of hydroxylamine nitrate and the utilization efficiency of the resin is 67 percent.
Comparative example
370mL of 007X 7 cation exchange resin which is subjected to acid activation treatment is added into an ion exchange column of phi 3.5X 40cm, and the ion exchange column is connected for standby by a device in the background technology.
Adding 682mL of 10% hydroxylamine sulfate solution into the ion exchange column from top to bottom at a flow rate of 11-12 mL/min, so that the adsorption residual liquid flows out from the bottom of the column, and carefully adjusting the discharge rate to keep the feed rate and the discharge rate of the ion exchange column consistent; after adsorption, adding pure water into the ion exchange column for washing in the manner until sulfate ions can not be detected in the washing liquid; then adjusting the flow rate to 5-6 mL/min, adding 152mL of nitric acid solution into the ion exchange column according to the feeding mode for elution, and continuously detecting the pH value of the eluent, wherein the pH value of the eluent is preferably not lower than 3.0; and finally, washing with pure water until the pH value of the water washing liquid is neutral. And (3) receiving the eluent and the water washing liquid with the pH value of more than 3.0, and detecting that the eluent and the water washing liquid contain 12g of hydroxylamine nitrate, wherein the resin utilization efficiency is 25.9%.
Claims (7)
1. An ion exchange device comprises an ion exchange column and a three-way valve, and is characterized in that a third three-way valve (h) is arranged at the bottom end of the ion exchange column, and an IV three-way valve (e) and a V three-way valve (f) are arranged at the top end of the ion exchange column; one end of the third three-way valve (h) is connected with a vent pipeline, and the other end of the third three-way valve (h) is connected with the second three-way valve (d); one end of the IV three-way valve (e) is connected with a vent pipeline, and the other end is connected with a discharge pipe (b); one end of the V-th three-way valve (f) is connected with a vent pipeline, and the other end of the V-th three-way valve (f) is connected with the I-th three-way valve (c); one end of the first three-way valve (c) is connected with the feeding pipe (a), the other end of the first three-way valve (c) is connected with the second three-way valve (d), and the other end of the second three-way valve (d) is connected with the discharging pipe (b); the I-th three-way valve (c) and the II-th three-way valve (d) are installed at the same height, and the IV-th three-way valve (e) and the V-th three-way valve (f) are installed at the same height and are higher than the I-th three-way valve (c) and the II-th three-way valve (d).
2. Ion exchange unit according to claim 1, characterised in that the function of the I three-way valve (c) is to switch the feed of starting hydroxylamine salt and elution acid; the function of the II three-way valve (d) is to switch the feeding of the hydroxylamine salt and the discharging of the eluent; the third three-way valve (h) is used for switching the feeding of the hydroxylamine salt as the raw material, the discharging of the eluent and the column emptying; the IV three-way valve (e) is used for switching the discharging and emptying of the adsorption residual liquid; the function of the V three-way valve (f) is to switch the elution acid feeding and emptying; and a pipeline between the II-th three-way valve (d) and the III-th three-way valve (h) is used as a feed pipe of the hydroxylamine salt raw material and a discharge pipe of the eluent.
3. An ion exchange process for preparing hydroxylamine nitrate or hydroxylamine perchlorate using the ion exchange apparatus of claim 1, comprising the steps of:
(1) adsorption: switching valves, adding metered hydroxylamine salt solution into the ion exchange column from bottom to top for adsorption through a first three-way valve (c), a second three-way valve (d) and a third three-way valve (h), and allowing the adsorption residual liquid to flow out of a discharge pipe through a fourth three-way valve (e);
(2) washing with water: washing the ion exchange column with pure water according to the feeding mode in the step (1) until no raw material hydroxylamine salt is detected in the washing liquid;
(3) and (3) elution: switching valves, adding metered aqueous solution of nitric acid or aqueous solution of perchloric acid into the ion exchange column from top to bottom through an I three-way valve (c) and a V three-way valve (f) for elution, enabling eluent to flow out of the bottom of the ion exchange column through a III three-way valve (h), turning upwards along a pipeline, passing through a II three-way valve (d), discharging and collecting the eluent through a discharging pipe;
(4) washing with water: washing the ion exchange column with pure water according to the feeding mode of the step (3) until the pH value of the effluent liquid is detected to be neutral;
and (4) effluent liquid of the steps (3) and (4) is diluted hydroxylamine nitrate or hydroxylamine perchlorate solution, and the product can be obtained after further concentration and crystallization.
4. The ion exchange process of claim 3, wherein the ion exchange column is packed with a cation exchange resin.
5. The ion exchange process of claim 4, wherein the cation exchange resin is of type 732 (001 x 7), 001 x 4, 001 x 8, Dowex-50, Amberlite IR-120, Lewatit-100.
6. The ion exchange process of claim 4, wherein the cation exchange resin is pre-acid activated.
7. The ion exchange process of claim 1 wherein the hydroxylamine salt solution is an aqueous solution of hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine oxalate or hydroxylamine phosphate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010041131.XA CN111111793B (en) | 2020-01-02 | 2020-01-02 | Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate |
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| CN202010041131.XA CN111111793B (en) | 2020-01-02 | 2020-01-02 | Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate |
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| CN111111793B CN111111793B (en) | 2023-09-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661126A (en) * | 2021-01-05 | 2021-04-16 | 浙江锦华新材料股份有限公司 | Preparation method of solid hydroxylamine hydrochloride |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3695834A (en) * | 1970-10-12 | 1972-10-03 | Atomic Energy Commission | Cation exchange conversion of hydroxylamine sulfate to hydroxylamine nitrate |
| US5762897A (en) * | 1996-05-03 | 1998-06-09 | Alliedsignal Inc. | Method for manufacturing hydroxylamine |
| CN1184077A (en) * | 1996-12-06 | 1998-06-10 | 陈淑奇 | Ion exchange process for producing potassium nitrate |
| CN109336998A (en) * | 2018-07-27 | 2019-02-15 | 浙江工业大学 | Macroporous ion-exchange resin and ion interchange unit for the absorption of high concentration rhenium |
| CN211755052U (en) * | 2020-01-02 | 2020-10-27 | 黎明化工研究设计院有限责任公司 | Ion exchange device |
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2020
- 2020-01-02 CN CN202010041131.XA patent/CN111111793B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3695834A (en) * | 1970-10-12 | 1972-10-03 | Atomic Energy Commission | Cation exchange conversion of hydroxylamine sulfate to hydroxylamine nitrate |
| GB1313439A (en) * | 1970-10-12 | 1973-04-11 | Atomic Energy Commission | Cation exchange conversion of hydroxylamine sulphate to hydroxylamine nitrate |
| US5762897A (en) * | 1996-05-03 | 1998-06-09 | Alliedsignal Inc. | Method for manufacturing hydroxylamine |
| CN1184077A (en) * | 1996-12-06 | 1998-06-10 | 陈淑奇 | Ion exchange process for producing potassium nitrate |
| CN109336998A (en) * | 2018-07-27 | 2019-02-15 | 浙江工业大学 | Macroporous ion-exchange resin and ion interchange unit for the absorption of high concentration rhenium |
| CN211755052U (en) * | 2020-01-02 | 2020-10-27 | 黎明化工研究设计院有限责任公司 | Ion exchange device |
Non-Patent Citations (3)
| Title |
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| 常志华,张香文,米镇涛: "离子交换法合成推进剂用高氯酸羟胺的研究" * |
| 张蒙蒙等: ""高氯酸羟胺的合成及表征"" * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661126A (en) * | 2021-01-05 | 2021-04-16 | 浙江锦华新材料股份有限公司 | Preparation method of solid hydroxylamine hydrochloride |
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