CN105692577A - Continuous dynamic polymerization large-scale production method for high-viscosity non-caking potassium polymetaphosphate - Google Patents
Continuous dynamic polymerization large-scale production method for high-viscosity non-caking potassium polymetaphosphate Download PDFInfo
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- CN105692577A CN105692577A CN201610088639.9A CN201610088639A CN105692577A CN 105692577 A CN105692577 A CN 105692577A CN 201610088639 A CN201610088639 A CN 201610088639A CN 105692577 A CN105692577 A CN 105692577A
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/44—Metaphosphates
- C01B25/445—Metaphosphates of alkali metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
The invention discloses a continuous dynamic polymerization large-scale production method for high-viscosity non-caking potassium polymetaphosphate.The method includes: adding a phosphorus containing material and a potassium containing material into a neutralizing tank, stirring for complete reaction, preparing neutralization liquid, and controlling a PH value in 3.0-5.0; transferring the liquid to a smelting furnace with a high-temperature-resistant corrosion-resistance liner directly or after concentration and crystallization or drying and dewatering, performing high-temperature melting at the temperature of 850-1000 DEG C; after materials in the smelting furnace is completely melted, discharging out of the smelting furnace, quickly cooling and solidifying, and grinding to 20 meshes below; transferring to a stainless steel rotary furnace for sintering reaction at the temperature of 450-650 DEG C for 0.5-2.0h, and discharging to obtain the high-viscosity non-caking potassium polymetaphosphate.The high-viscosity non-caking potassium polymetaphosphate can be produced by existing conventional phosphate production equipment, and high efficiency, method simplicity and convenience in implementation are realized.
Description
Technical field
The present invention relates to the production method of a kind of Kurrol's salt, what be specifically related to that a kind of high viscosity do not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously。
Technical background
Kurrol's salt is otherwise known as Rule potassium salt, potassium polyphposphate, potassium metaphosphate, and its molecular formula is: KPO3Or (KPO3) n, sterling contains 39.87% potassium oxide and 60.13% phosphorus pentoxide, for the straight chain type Quadrafos of high polymeric, has three potassium metaphosphates of a small amount of structure in the form of a ring and four potassium metaphosphates etc. of circulus to exist；Outward appearance is the colourless block to white glassy or sheet, or is white fibrous crystallization or powder, relative density (25 DEG C) 2.893, fusing point 807 DEG C, and boiling point 1320 DEG C is slightly soluble in cold water, is soluble in sodium salt solution and forms viscosity solution。Kurrol's salt is a kind of important food additive, and as Food Texture modifying agent, food is remained stable for by Kurrol's salt, homogeneous matter structure and good outward appearance play a role, and viscosity is its important indicator played a role。
In the '30s later stage in last century, TVA company phosphorus pentoxide carries out following reaction under the high temperature of 890～900 DEG C with powdery potassium chloride and water and makes:
P2O5+2KCl+H2O=2KPO3+2HCl
Washing the HCl gas of heat in packed tower with water, to absorb unreacted phosphorus pentoxide, the phosphoric acid of generation returns to reative cell。Then in reactor, release melted Kurrol's salt。In the sixties in last century, TVA company at the temperature of 930 DEG C, reacts phosphoric acid by wet process and potassium chloride 30 minutes and has produced Kurrol's salt。In succession occur in that again SAI method, EMC method, combustion method etc. later, all produce for raw materials melt or sintering with phosphoric acid and potassium chloride for raw material or with element phosphor and potassium chloride。
" production method of Kurrol's salt and the equipment of production " of Chinese invention patent application publication No. CN102897740A and Chinese invention patent application publication No. CN102910610A, CN103663402A " preparation method of high-viscosity potassium metaphosphate " are a kind of sintering process, this method is only suitable for batch (-type) small lot batch manufacture on a small scale, owing to being static polymerization, the half-cooked easy caking of response time length, product, efficiency is low, labor intensity is big, and ceramic utensil unavoidable loss is very big and adheres to many products and abandons therewith。
It was verified that the Kurrol's salt produced of fusion method is only small due to the reason viscosity of molecular structure, without value in food industry；And sintering process is owing to solidifying, with the rising of temperature, the process hardened after having low temperature softening partial melting at about 200 DEG C in course of reaction; it requires height to consersion unit is corrosion-resistant; and material can not dynamic aggregation; response time is long; the half-cooked easy caking of product, although full-bodied product can be produced and be but difficult to continuous large-scale production。
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of high viscosity do not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, be prepared as follows:
By phosphorous raw material with add in neutralization chamber containing potassium raw material and stir, fully after reaction, preparation neutralizes feed liquid, and pH value controls at 3.0-5.0；It is transferred in the smelting furnace with corrosion-and high-temp-resistant liner by neutralizing feed liquid again, carrying out high-temperature fusion, melt temperature controls at 850-1000 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at 450-650 DEG C, sintering time controls after 0.5-2.0h, discharge, namely prepares high viscosity and does not lump Kurrol's salt。
Described phosphorous raw material refers to phosphoric acid and/or phosphorus pentoxide。
The described raw material containing potassium refers to potassium hydroxide and/or potassium carbonate and/or potassium chloride。
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
Described melt temperature controls at 850-950 DEG C。
Described sintering temperature controls at 500-600 DEG C。
The material of described rustless steel rotary furnace can be 321,316L, the rustless steel of 310S model。
Described neutralization feed liquid is before being transferred to smelting furnace, it is also possible to by after neutralizing the concentrated crystallization of feed liquid or transfer to smelting furnace after drying dehydration and carry out frit reaction。
Described neutralization feed liquid can also substitute with potassium dihydrogen phosphate。
Beneficial effects of the present invention: the method is the new method combined with sintering process by fusion method; it solve fusion method product viscosity low; sintering process to consersion unit corrosion-resistant require high, material can not dynamic aggregation, response time length, half-cooked easy caking, process consumptive material high with supplies consumption, can not the shortcoming of scale quantity-produced, it is achieved thereby that can the good product mobility of dynamic aggregation large-scale production and preparation continuously not the luming of high-viscosity potassium metaphosphate。Using existing phosphate conventional equipment (the common sodium hexameta phosphate smelting furnace of melting process, the common sodium tripolyphosphate rotary furnace of sintering process) just can produce, efficiency is high, method is simple, and it is convenient to implement。
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described。
Embodiment 1
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
The rustless steel that material is 310S model of the described rustless steel rotary furnace for sintering reaction。
Being added in neutralization chamber with potassium hydroxide by phosphoric acid and stir, fully after reaction, control ph is about 3.0；Again feed liquid is directly transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carrying out high-temperature fusion, melt temperature controls at about 850 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at about 650 DEG C, sintering time controls after about 2.0h, discharge, namely prepares high-viscosity potassium metaphosphate。Viscosity is 122.0CPS after testing, and good product mobility is not lumpd。
Embodiment 2
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
The rustless steel that material is 316L model of the described rustless steel rotary furnace for sintering reaction。
Being added in neutralization chamber with potassium carbonate by phosphoric acid and stir, fully after reaction, control ph is about 4.0；To be transferred to after concentrated for feed liquid crystallization in the smelting furnace with corrosion-and high-temp-resistant liner again, carrying out high-temperature fusion, melt temperature controls at about 930 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at about 600 DEG C, sintering time controls after about 1.5h, discharge, namely prepares high-viscosity potassium metaphosphate。Viscosity is 52.2CPS after testing, and good product mobility is not lumpd。
Embodiment 3
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
The rustless steel that material is 321 models of the described rustless steel rotary furnace for sintering reaction。
Being added in neutralization chamber with potassium carbonate by phosphorus pentoxide and stir, fully after reaction, control ph is about 5.0；To be transferred to after feed liquid drying dehydration in the smelting furnace with corrosion-and high-temp-resistant liner again, carrying out high-temperature fusion, melt temperature controls at about 1000 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at about 450 DEG C, sintering time controls after about 0.5h, discharge, namely prepares high-viscosity potassium metaphosphate。Viscosity is 16.8CPS after testing, and good product mobility is not lumpd。
Embodiment 4
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
The rustless steel that material is 321 models of the described rustless steel rotary furnace for sintering reaction。
Being added in neutralization chamber with potassium chloride by phosphorus pentoxide and stir, fully after reaction, control ph is about 3.5；Again feed liquid is directly transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carrying out high-temperature fusion, melt temperature controls at about 900 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at about 560 DEG C, sintering time controls after about 1h, discharge, namely prepares high-viscosity potassium metaphosphate。Viscosity is 68.3CPS after testing, and good product mobility is not lumpd。
Embodiment 5
The described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
The rustless steel that material is 321 models of the described rustless steel rotary furnace for sintering reaction。
Potassium dihydrogen phosphate is transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carrying out high-temperature fusion, melt temperature controls at about 950 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at about 500 DEG C, sintering time controls after about 1h, discharge, namely prepares high-viscosity potassium metaphosphate。Viscosity is 28.8CPS after testing, and good product mobility is not lumpd。
Claims (9)
1. what high viscosity did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: it is prepared as follows:
By phosphorous raw material with add in neutralization chamber containing potassium raw material and stir, fully after reaction, preparation neutralizes feed liquid, and pH value controls at 3.0-5.0；It is transferred in the smelting furnace with corrosion-and high-temp-resistant liner by neutralizing feed liquid again, carrying out high-temperature fusion, melt temperature controls at 850-1000 DEG C, when in smelting furnace, material is complete molten condition, discharge smelting furnace, rapid cooling curing, size-reduced to 20 orders, transfer to and rustless steel rotary furnace is sintered reaction, sintering temperature controls at 450-650 DEG C, sintering time controls after 0.5-2.0h, discharge, namely prepares high viscosity and does not lump Kurrol's salt。
2. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: described phosphorous raw material refers to phosphoric acid and/or phosphorus pentoxide。
3. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: the described raw material containing potassium refers to potassium hydroxide and/or potassium carbonate and/or potassium chloride。
4. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: the described smelting furnace with corrosion-and high-temp-resistant liner is the smelting furnace that liner is built into by zirconia block。
5. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: described melt temperature controls at 850-950 DEG C。
6. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: described sintering temperature controls at 500-600 DEG C。
7. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: the material of described rustless steel rotary furnace can be 321,316L, the rustless steel of 310S model。
8. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously; it is characterized in that: described neutralization feed liquid is before being transferred to smelting furnace, it is also possible to by after neutralizing the concentrated crystallization of feed liquid or transfer to smelting furnace after drying dehydration and carry out frit reaction。
9. what high viscosity according to claim 1 did not lump Kurrol's salt can dynamic aggregation large-scale method for producing continuously, it is characterised in that: described neutralization feed liquid can also substitute with potassium dihydrogen phosphate。
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| CN201510754652 | 2015-11-09 | ||
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385318A (en) * | 2022-09-29 | 2022-11-25 | 云南莱德福科技有限公司 | Preparation method of water-soluble potassium polymetaphosphate |
| WO2022257269A1 (en) * | 2021-06-11 | 2022-12-15 | 云南莱德福科技有限公司 | Slow-dissolving compound fertilizer containing potassium polyphosphate, preparation method therefor, and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53113800A (en) * | 1977-03-17 | 1978-10-04 | Mitsubishi Chem Ind Ltd | Production of potassium polymetaphosphate |
| EP0351281A1 (en) * | 1988-07-13 | 1990-01-17 | Rhone-Poulenc Chimie | Process for the preparation of phosphates by fusion |
| CN1054055A (en) * | 1990-01-16 | 1991-08-28 | E.I.内穆尔杜邦公司 | Metaphosphate glass composition |
| CN1208717A (en) * | 1997-08-05 | 1999-02-24 | 味之素株式会社 | Process for producing alkali metal polyphosphates |
| CN103663402A (en) * | 2012-11-14 | 2014-03-26 | 云南莱德福科技有限公司 | Preparation method for high-viscosity potassium metaphosphate |
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2016
- 2016-02-17 CN CN201610088639.9A patent/CN105692577B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53113800A (en) * | 1977-03-17 | 1978-10-04 | Mitsubishi Chem Ind Ltd | Production of potassium polymetaphosphate |
| EP0351281A1 (en) * | 1988-07-13 | 1990-01-17 | Rhone-Poulenc Chimie | Process for the preparation of phosphates by fusion |
| CN1054055A (en) * | 1990-01-16 | 1991-08-28 | E.I.内穆尔杜邦公司 | Metaphosphate glass composition |
| CN1208717A (en) * | 1997-08-05 | 1999-02-24 | 味之素株式会社 | Process for producing alkali metal polyphosphates |
| CN103663402A (en) * | 2012-11-14 | 2014-03-26 | 云南莱德福科技有限公司 | Preparation method for high-viscosity potassium metaphosphate |
Non-Patent Citations (1)
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| 陈嘉甫: "《磷酸盐的生产与应用》", 31 December 1989, 成都科技大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022257269A1 (en) * | 2021-06-11 | 2022-12-15 | 云南莱德福科技有限公司 | Slow-dissolving compound fertilizer containing potassium polyphosphate, preparation method therefor, and application thereof |
| CN115385318A (en) * | 2022-09-29 | 2022-11-25 | 云南莱德福科技有限公司 | Preparation method of water-soluble potassium polymetaphosphate |
| CN115385318B (en) * | 2022-09-29 | 2023-05-09 | 云南莱德福科技有限公司 | Preparation method of water-soluble potassium polymetaphosphate |
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Denomination of invention: Continuous dynamic polymerization and large scale production of high viscosity non caking potassium polymetaphosphate Effective date of registration: 20210512 Granted publication date: 20171110 Pledgee: Xuzhou Productivity Promotion Center Pledgor: XUZHOU HENS FOODS Co.,Ltd. Registration number: Y2021980003524 |
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Address after: 221011 south side of Xujia Expressway in Xuzhou Industrial Park, Jiangsu Province Patentee after: Jiangsu Hengshi Food Technology Co.,Ltd. Address before: 221011 south side of Xujia Expressway in Xuzhou Industrial Park, Jiangsu Province Patentee before: XUZHOU HENS FOODS CO.,LTD. |