CN105692577B - What high viscosity did not lumpd potassium metapbosphate can continuous dynamic aggregation large-scale method for producing - Google Patents
What high viscosity did not lumpd potassium metapbosphate can continuous dynamic aggregation large-scale method for producing Download PDFInfo
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- CN105692577B CN105692577B CN201610088639.9A CN201610088639A CN105692577B CN 105692577 B CN105692577 B CN 105692577B CN 201610088639 A CN201610088639 A CN 201610088639A CN 105692577 B CN105692577 B CN 105692577B
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- 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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- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
Do not lumpd the invention discloses high viscosity potassium metapbosphate can continuous dynamic aggregation large-scale method for producing, phosphorous raw material is added in neutralization chamber and stirred with raw material containing potassium by this method, fully after reaction, is prepared and is neutralized feed liquid, pH value is controlled 3.0 5.0；Again by feed liquid is direct or concentrated crystallization after or be transferred in the smelting furnace with corrosion-and high-temp-resistant liner after drying and dehydrating, high-temperature fusion is carried out, melting temperature is controlled at 850 1000 DEG C, when material in smelting furnace is in complete molten condition, discharge smelting furnace, rapid cooling and solidifying, through being crushed to below 20 mesh, transfers in stainless steel rotary furnace and is sintered reaction, sintering temperature is controlled at 450 650 DEG C, sintering time is controlled after 0.5 2.0 h, discharge, that is, high viscosity is made and does not lump potassium metapbosphate；The present invention can be produced using existing phosphate conventional equipment, and efficiency high, method are simple, easy to implement.
Description
Technical field
The present invention relates to a kind of production method of potassium metapbosphate, and in particular to a kind of high viscosity is not lumpd potassium metapbosphate
Can continuous dynamic aggregation large-scale method for producing.
Technical background
Potassium metapbosphate is otherwise known as Rule sylvite, potassium polyphposphate, potassium metaphosphate, and its molecular formula is：KPO3Or（KPO3) n,
Sterling contains 39.87% potassium oxide and 60.13% phosphorus pentoxide, is the straight chain type Quadrafos of high polymeric, and it is in ring to have a small amount of
Three potassium metaphosphates of shape structure and four potassium metaphosphates of cyclic structure etc. are present；Outward appearance in the colourless block to white glassy or
Piece, or for white fibrous crystallization or powder, relative density（25℃）2.893,807 DEG C of fusing point, 1320 DEG C of boiling point, it is slightly soluble in cold
Water, it is soluble in sodium salt solution and forms viscosity solution.Potassium metapbosphate is a kind of important food additives, as Food Texture
Modifying agent, potassium metapbosphate keep stable, homogeneous texture and good outward appearance to play a role to food, and viscosity is its performance
The important indicator of effect.
In the '30s later stage in last century, TVA companies phosphorus pentoxide is with powdery potassium chloride and water at 890~900 DEG C
At a high temperature of carry out it is following reaction and it is manufactured：
P2O5 +2KCl+ H2O=2KPO3+2HCl
The HCl gas of heat is washed with water in packed tower, to absorb unreacted phosphorus pentoxide, the phosphoric acid of generation returns
Return to reative cell.Then the potassium metapbosphate of melting is released out of reactor.In the sixties in last century, TVA companies are wet method
Phosphoric acid at a temperature of 930 DEG C, reacts 30 minutes with potassium chloride and has produced potassium metapbosphate.Later and there is SAI in succession
Method, EMC methods, combustion method etc., all it is using phosphoric acid and potassium chloride as raw material or using element phosphor and potassium chloride as raw materials melt or sintering
Produce.
The A of Chinese invention patent application publication No. CN 102897740 " production method of potassium metapbosphate and production are set
It is standby " and the 103663402 A " systems of high-viscosity potassium metaphosphate of A, CN of Chinese invention patent application publication No. CN 102910610
Preparation Method " is a kind of sintering process, and this method is only suitable for small-scale batch (-type) small lot production, due to being static polymerization, reaction
Time is long, product is half-cooked easily lumps, and efficiency is low, and labor intensity is big, and ceramic utensil unavoidable loss is very big and adheres to not
Few product abandons therewith.
It was verified that the potassium metapbosphate produced of fusion method viscosity very little due to molecular structure, in food
Industrially without value；And sintering process in course of reaction at 200 DEG C or so due to having after low temperature softening partial melting with temperature
Rise solidify hardened process again, it is corrosion-resistant to consersion unit to require high, and material is unable to dynamic aggregation, reaction time
It is long, the half-cooked easily caking of product, although can produce highly viscous product is difficult to continuous large-scale production.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides a kind of high viscosity do not lump potassium metapbosphate can
Continuous dynamic aggregation large-scale method for producing, is prepared as follows：
Phosphorous raw material is added in neutralization chamber and stirred with raw material containing potassium, fully after reaction, prepares and neutralizes feed liquid, pH value control
System is in 3.0-5.0；Feed liquid will be neutralized again to be transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carries out high-temperature fusion, melting
Temperature control is at 850-1000 DEG C, when material in smelting furnace is in complete molten condition, discharges smelting furnace, rapid cooling and solidifying, through powder
It is broken to below 20 mesh, transfers in stainless steel rotary furnace and be sintered reaction, sintering temperature is controlled at 450-650 DEG C, sintering
Time control is made high viscosity and not lumpd potassium metapbosphate after 0.5-2.0 h, discharge.
Described phosphorous raw material refers to phosphoric acid and/or phosphorus pentoxide.
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 melting temperature is controlled at 850-950 DEG C.
Described sintering temperature is controlled at 500-600 DEG C.
The material of described stainless steel rotary furnace can be the stainless steel of 321,316L, 310S models.
Described neutralization feed liquid will can also be neutralized after the concentrated crystallization of feed liquid or de- through drying before smelting furnace is transferred to
Smelting furnace is transferred to after water and carries out frit reaction.
Described neutralization feed liquid can also be substituted with potassium dihydrogen phosphate.
Beneficial effects of the present invention：This method is the new method for being combined fusion method with sintering process, and it solves melting
Method product viscosity is low, and sintering process requirement corrosion-resistant to consersion unit is high, material is unable to dynamic aggregation, the reaction time is long, half-cooked easy
Caking, process consumptive material and supplies consumption are high, are unable to the shortcomings that scale quantity-produced, it is achieved thereby that high viscosity poly-metaphosphoric acid
Potassium the good product mobility of dynamic aggregation large-scale production and preparation can not lump continuously.Routinely set using existing phosphate
It is standby（Melting process common calgon smelting furnace, the common sodium tripolyphosphate rotary furnace of sintering process）It can be produced,
Efficiency high, method are simple, easy to implement.
Embodiment
With reference to 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 material of the described stainless steel rotary furnace for sintering reaction is the stainless steel of 310S models.
Phosphoric acid is added in neutralization chamber and stirred with potassium hydroxide, fully after reaction, control ph is 3.0 or so；Again will
Feed liquid is directly transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carries out high-temperature fusion, and melting temperature is controlled on 850 DEG C of left sides
The right side, when material in smelting furnace is in complete molten condition, smelting furnace is discharged, rapid cooling and solidifying, through being crushed to below 20 mesh, is retransferred
Reaction is sintered into stainless steel rotary furnace, at 650 DEG C or so, sintering time is controlled in 2.0 h or so for sintering temperature control,
After discharge, that is, high-viscosity potassium metaphosphate is made.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 material of the described stainless steel rotary furnace for sintering reaction is the stainless steel of 316L models.
Phosphoric acid is added in neutralization chamber and stirred with potassium carbonate, fully after reaction, control ph is 4.0 or so；Again will material
It is transferred to after the concentrated crystallization of liquid in the smelting furnace with corrosion-and high-temp-resistant liner, carries out high-temperature fusion, melting temperature control exists
930 DEG C or so, when material in smelting furnace is in complete molten condition, discharge smelting furnace, rapid cooling and solidifying, through be crushed to 20 mesh with
Under, transfer in stainless steel rotary furnace and be sintered reaction, at 600 DEG C or so, sintering time control exists for sintering temperature control
1.5 h or so, after discharge, that is, high-viscosity potassium metaphosphate is made.Viscosity is 52.2CPS after testing, and good product mobility is not tied
Block.
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 material of the described stainless steel rotary furnace for sintering reaction is the stainless steel of 321 models.
Phosphorus pentoxide is added in neutralization chamber and stirred with potassium carbonate, fully after reaction, control ph is 5.0 or so；
Feed liquid is transferred to after drying and dehydrating in the smelting furnace with corrosion-and high-temp-resistant liner again, carries out high-temperature fusion, melting temperature
Control is at 1000 DEG C or so, when material in smelting furnace is in complete molten condition, discharges smelting furnace, rapid cooling and solidifying, through being crushed to
Below 20 mesh, transfer in stainless steel rotary furnace and be sintered reaction, sintering temperature control is at 450 DEG C or so, sintering time
Control is in 0.5 h or so, after discharge, i.e., obtained high-viscosity potassium metaphosphate.Viscosity is 16.8CPS after testing, product mobility
It is good not lump.
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 material of the described stainless steel rotary furnace for sintering reaction is the stainless steel of 321 models.
Phosphorus pentoxide is added in neutralization chamber and stirred with potassium chloride, fully after reaction, control ph is 3.5 or so；
Feed liquid is directly transferred in the smelting furnace with corrosion-and high-temp-resistant liner again, carries out high-temperature fusion, melting temperature is controlled 900
DEG C or so, when material in smelting furnace is in complete molten condition, smelting furnace is discharged, it is rapid to cool and solidify, through being crushed to below 20 mesh, then
It is transferred in stainless steel rotary furnace and is sintered reaction, at 560 DEG C or so, sintering time control is left in 1 h for sintering temperature control
The right side, after discharge, that is, high-viscosity potassium metaphosphate is made.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 material of the described stainless steel rotary furnace for sintering reaction is the stainless steel of 321 models.
Potassium dihydrogen phosphate is transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carries out high-temperature fusion, melting temperature
Control is at 950 DEG C or so, when material in smelting furnace is in complete molten condition, discharges smelting furnace, rapid cooling and solidifying, through being crushed to 20
Below mesh, transfer in stainless steel rotary furnace and be sintered reaction, sintering temperature control is at 500 DEG C or so, sintering time control
System is in 1 h or so, after discharge, i.e., obtained high-viscosity potassium metaphosphate.Viscosity is 28.8CPS after testing, and good product mobility is not
Caking.
Claims (2)
1. high viscosity is not lumpd, potassium metapbosphate can continuous dynamic aggregation large-scale method for producing, it is characterised in that by as follows
It is prepared by method：
Phosphorous raw material is added in neutralization chamber and stirred with raw material containing potassium, fully after reaction, prepares and neutralizes feed liquid, the control of pH values
5.0；Feed liquid will be neutralized again to be transferred in the smelting furnace with corrosion-and high-temp-resistant liner, carries out high-temperature fusion, melting temperature control
System at 1000 DEG C, when material in smelting furnace be in complete molten condition, discharge smelting furnace, rapidly cool and solidify, through be crushed to 20 mesh with
Under, transferring in stainless steel rotary furnace and be sintered reaction, at 450 DEG C, sintering time is controlled in 0.5h for sintering temperature control,
After discharge, that is, high viscosity is made and does not lump potassium metapbosphate；
Described phosphorous raw material refers to phosphorus pentoxide；
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；
The material of described stainless steel rotary furnace is the stainless steel of 321,316L, 310S models；
Described neutralization feed liquid will also be neutralized after the concentrated crystallization of feed liquid or turned again after drying and dehydrating before smelting furnace is transferred to
Move to smelting furnace and carry out frit reaction.
2. the method as described in claim 1, it is characterised in that：Described neutralization feed liquid is substituted with potassium dihydrogen phosphate.
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| CN2015107546529 | 2015-11-09 | ||
| CN201510754652 | 2015-11-09 |
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| CN113292360B (en) * | 2021-06-11 | 2022-04-29 | 云南莱德福科技有限公司 | Potassium polyphosphate slow-soluble compound fertilizer and preparation method and application thereof |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53113800A (en) * | 1977-03-17 | 1978-10-04 | Mitsubishi Chem Ind Ltd | Production of potassium polymetaphosphate |
| FR2634191B1 (en) * | 1988-07-13 | 1991-12-27 | Rhone Poulenc Chimie | PROCESS FOR THE PREPARATION OF PHOSPHATES BY MELTING |
| US5196381A (en) * | 1990-01-16 | 1993-03-23 | E. I. Du Pont De Nemours And Company | Metaphosphate glass composition |
| JP3695072B2 (en) * | 1997-08-05 | 2005-09-14 | 味の素株式会社 | Method for producing alkali metal condensed phosphate |
| CN102910610A (en) * | 2012-11-14 | 2013-02-06 | 云南莱德福科技有限公司 | Method for preparing high viscosity 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. |