CN106146553A - A kind of preparation method of hexapotassium potassium salt - Google Patents
A kind of preparation method of hexapotassium potassium salt Download PDFInfo
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- CN106146553A CN106146553A CN201510173737.8A CN201510173737A CN106146553A CN 106146553 A CN106146553 A CN 106146553A CN 201510173737 A CN201510173737 A CN 201510173737A CN 106146553 A CN106146553 A CN 106146553A
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Abstract
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of with short production cycle, production efficiency is high, the hexapotassium potassium salt that production cost is low.With hexamethylene diamine, hydrochloric acid, phosphorous acid, formaldehyde, potassium hydroxide and appropriate water as raw material, the method comprises the following steps: added by hexamethylene diamine in the reactor sealed, control temperature 40～50 DEG C, supercharging in reactor, making the atmospheric pressure in reactor is 1.5～3 normal atmospheres, dropping hydrochloric acid, and be slowly stirred；Hydrochloric acid drips in phosphorous acid high-pressure pump suction reactor and be stirred continuously after finishing；Lifting temperature to 80～110 DEG C and be slowly added dropwise formaldehyde, the atmospheric pressure in reactor is adjusted to 1 normal atmosphere, sprays into potassium hydroxide solution, making the pH value of liquid in reactor is 6～8, lowers the temperature, blowing after chemical examination is qualified.
Description
Technical field:
The present invention relates to the preparation method of hexapotassium potassium salt, belong to circulating water treatment technology field.
Background technology:
Hexapotassium potassium salt appearance colorless, to slightly yellow transparency liquid, has the highest dissolubility, can stop in water
Dirt salt formed incrustation scale, be good calcium sulfate antisludging agent, especially suitable high-alkali high pH condition, be particularly adapted to boiler water process,
The antisludging agent of reverse osmosis membrane.The quality index of hexapotassium potassium salt is: appearance colorless is to slightly yellow transparent, and liquid is lived
Property component (in terms of acid) %21.2～24.6 active constituents (in terms of salt) %31.0～36.0 chlorides (in terms of Cl-) %≤4.0 are total
Phosphorus (in terms of P043-) content % >=16.8 phosphorous (in terms of P033-) content %≤2.0Fe (in terms of Fe3+) content ppm≤
35 density (20 DEG C) g/cm3 1.21～1.31PH value (1% aqueous solution) 6.0～8.0.Traditional mode of production hexapotassium potassium salt
The technique production cycle long, production efficiency is low, and production cost is high, and the stability of properties of product is relatively low.
Summary of the invention:
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of with short production cycle, production efficiency is high, production cost
Low hexapotassium potassium salt.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of preparation method of hexapotassium potassium salt, with hexamethylene diamine, hydrochloric acid, phosphorous acid, formaldehyde, potassium hydroxide and
Appropriate water is raw material, and the method comprises the following steps:
(1) being added by hexamethylene diamine in the reactor sealed, control temperature 40～70 DEG C, supercharging in reactor, in making reactor
Atmospheric pressure is 1.5～3 normal atmospheres, drips hydrochloric acid, and is slowly stirred；
(2) by phosphorous acid high-pressure pump suction reactor and be stirred continuously, until stirring after hydrochloric acid drips and finishes；
(3) lifting temperature to 80～110 DEG C and be slowly added dropwise formaldehyde, and be constantly stirred, mixing speed is 60～80 turns every point, drips off
It is incubated 3～4 hours；Remove the impurity in material.
(4) during insulation, adding appropriate water with potassium hydroxide, to be configured to potassium hydroxide solution stand-by；
(5), after insulation terminates, the atmospheric pressure in reactor is adjusted to 1 normal atmosphere, then sprays into step (4) institute with spray
The potassium hydroxide solution being configured to, in order to adjust the pH value of liquid in reactor, makes and is constantly stirred, constantly chemically examining, directly
To reactor, the pH value of liquid is 6～8；
(6) cooling, blowing.
The material mass ratio of hexamethylene diamine, hydrochloric acid, phosphorous acid, formaldehyde and the potassium hydroxide solution described in above-mentioned steps (1)～(5) is
2: 5: 10: 6～7: 6～7.
The hydrochloric acid solution that hydrochloric acid is 30% described in above-mentioned steps (1).
The phosphorous acid solution that phosphorous acid is 65% described in above-mentioned steps (2).
Potassium hydroxide described in above-mentioned steps (4) is 9: 10 with the material mass ratio of water.
It is an advantage of the invention that with short production cycle, production efficiency is high, and production cost is low, operates safety, energy-conserving and environment-protective, production capacity
Greatly, it is easy to industrialized production.The product quality produced through the present invention is high, and performance is more stable.
Detailed description of the invention:
Below by specific embodiment, technical scheme is described in further detail, but the present invention is not limited to
These embodiments.
Embodiment 1
(1) 300kg hexamethylene diamine is added in the reactor sealed, control temperature 40～70 DEG C, supercharging in reactor, make reaction
Atmospheric pressure in still is 1.5 normal atmospheres, the hydrochloric acid 750kg of dropping 30%, and is slowly stirred；
(2) by the phosphorous acid solution 1500kg high-pressure pump suction reactor of 65% and be stirred continuously, until stirring after hydrochloric acid drips and finishes
Mix uniformly；
(3) lifting temperature to 80～110 DEG C and be slowly added dropwise formaldehyde 1000kg, and be constantly stirred, mixing speed is 60～80 turns every point,
It is incubated 3.5 hours, removes the impurity in material；
(4) during insulation, adding water with potassium hydroxide, it is stand-by to be configured to potassium hydroxide solution 1000kg, wherein potassium hydroxide
It is 9: 10 with the ratio of water；
(5), after insulation terminates, the atmospheric pressure in reactor is adjusted to 1 normal atmosphere, then sprays into step (4) institute with spray
The potassium hydroxide solution being configured to, in order to adjust the pH value of liquid in reactor, makes and is constantly stirred, constantly chemically examining, directly
To reactor, the pH value of liquid is 6～8；
(6) cooling, blowing.
Embodiment 2
(1) 400kg hexamethylene diamine is added in the reactor sealed, control temperature 40～50 DEG C, supercharging in reactor, make reaction
Atmospheric pressure in still is 2 normal atmospheres, the hydrochloric acid 1000kg of dropping 30%, and is slowly stirred；
(2) by the phosphorous acid solution 2000kg high-pressure pump suction reactor of 65% and be stirred continuously, until stirring after hydrochloric acid drips and finishes
Mix uniformly；
(3) lifting temperature to 80～110 DEG C and be slowly added dropwise formaldehyde 1300kg, and be constantly stirred, mixing speed is 60～80 turns every point,
It is incubated 3.5 hours；
(4) during insulation, adding water with potassium hydroxide, it is stand-by to be configured to potassium hydroxide solution 1300kg, wherein potassium hydroxide
It is 9: 10 with the ratio of water；
(5), after insulation terminates, the atmospheric pressure in reactor is adjusted to 1 normal atmosphere, then sprays into step (4) institute with spray
The potassium hydroxide solution being configured to, in order to adjust the pH value of liquid in reactor, makes and is constantly stirred, constantly chemically examining, directly
To reactor, the pH value of liquid is 6～8；
(6) cooling, blowing.
Claims (5)
1. a preparation method for hexapotassium potassium salt, with hexamethylene diamine, hydrochloric acid, phosphorous acid, formaldehyde, potassium hydroxide and appropriate water as raw material, it is characterised in that: the method comprises the following steps:
(1) being added by hexamethylene diamine in the reactor sealed, control temperature 40～50 DEG C, supercharging in reactor, making the atmospheric pressure in reactor is 1.5～3 normal atmospheres, drips hydrochloric acid, and is slowly stirred；
(2) by phosphorous acid high-pressure pump suction reactor and be stirred continuously, until stirring after hydrochloric acid drips and finishes；
(3) lifting temperature to 80～110 DEG C and be slowly added dropwise formaldehyde, and be constantly stirred, mixing speed is 60～80 turns every point, is incubated 3-4 hour；
(4) during insulation, adding appropriate water with potassium hydroxide, to be configured to potassium hydroxide solution stand-by；
(5) after insulation terminates, atmospheric pressure in reactor is adjusted to 1 normal atmosphere, then spray into, with spray, the potassium hydroxide solution that step (4) is configured to, in order to adjust the pH value of liquid in reactor, make and be constantly stirred, constantly chemical examination, until the pH value of liquid is 6～8 in reactor；
(6) cooling, blowing.
The preparation method of hexapotassium potassium salt the most according to claim 1, it is characterised in that: the material mass ratio of hexamethylene diamine, hydrochloric acid, phosphorous acid, formaldehyde and the potassium hydroxide solution described in step (1)～(5) is 2: 5: 10: 6～7: 6～7.
The preparation method of hexapotassium potassium salt the most according to claim 1, it is characterised in that: the hydrochloric acid solution that hydrochloric acid is 30% described in step (1).
The preparation method of hexapotassium potassium salt the most according to claim 1, it is characterised in that: the phosphorous acid solution that phosphorous acid is 65% described in step (2).
The preparation method of hexapotassium potassium salt the most according to claim 1, it is characterised in that: the potassium hydroxide described in step (4) is 9: 10 with the material mass ratio of water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173737.8A CN106146553A (en) | 2015-04-09 | 2015-04-09 | A kind of preparation method of hexapotassium potassium salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173737.8A CN106146553A (en) | 2015-04-09 | 2015-04-09 | A kind of preparation method of hexapotassium potassium salt |
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| CN106146553A true CN106146553A (en) | 2016-11-23 |
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| CN201510173737.8A Pending CN106146553A (en) | 2015-04-09 | 2015-04-09 | A kind of preparation method of hexapotassium potassium salt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276441A (en) * | 2018-01-31 | 2018-07-13 | 山东大学 | The preparation method of two methylenephosphonic acid of cyclohexylamine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229618A (en) * | 2011-04-26 | 2011-11-02 | 河南清水源科技股份有限公司 | Hexamethylenediamine tetramethylene phosphonic acid disodium salt and its production process |
| CN103420507A (en) * | 2012-05-25 | 2013-12-04 | 鲍宜仿 | Preparation method of hexapotassium salt compound scale inhibitor |
| CN103420511A (en) * | 2012-05-25 | 2013-12-04 | 魏从莲 | Preparation method of diethylenetriamine penta (methylene phosphonic acid) sodium compound scale inhibitor |
-
2015
- 2015-04-09 CN CN201510173737.8A patent/CN106146553A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229618A (en) * | 2011-04-26 | 2011-11-02 | 河南清水源科技股份有限公司 | Hexamethylenediamine tetramethylene phosphonic acid disodium salt and its production process |
| CN103420507A (en) * | 2012-05-25 | 2013-12-04 | 鲍宜仿 | Preparation method of hexapotassium salt compound scale inhibitor |
| CN103420511A (en) * | 2012-05-25 | 2013-12-04 | 魏从莲 | Preparation method of diethylenetriamine penta (methylene phosphonic acid) sodium compound scale inhibitor |
Non-Patent Citations (1)
| Title |
|---|
| DIDIER VILLEMIN ET AL.: "Green Synthesis of Poly aminomethylenephosphonic Acids", 《PHOSPHORUS, SULFUR, AND SILICON》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276441A (en) * | 2018-01-31 | 2018-07-13 | 山东大学 | The preparation method of two methylenephosphonic acid of cyclohexylamine |
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Address after: Shandong City, Zaozhuang province 277100 City District Xi Wang Zhuang Township resident Applicant after: Shandong Xintai water treatment technology Limited by Share Ltd Address before: Shandong City, Zaozhuang province 277100 City District Xi Wang Zhuang Township resident Applicant before: Shandong Xin Tai water technology company limited |
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Application publication date: 20161123 |
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