CN102001639B - Method for continuously producing potassium pyrophosphate by two-step process - Google Patents
Method for continuously producing potassium pyrophosphate by two-step process Download PDFInfo
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- CN102001639B CN102001639B CN2010105246033A CN201010524603A CN102001639B CN 102001639 B CN102001639 B CN 102001639B CN 2010105246033 A CN2010105246033 A CN 2010105246033A CN 201010524603 A CN201010524603 A CN 201010524603A CN 102001639 B CN102001639 B CN 102001639B
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Abstract
The invention discloses a method for continuously producing potassium pyrophosphate by a two-step process, which comprises the following steps of: reacting phosphoric acid and potassium hydroxide in a neutralization kettle to obtain solution of dipotassium phosphate; spraying or depositing the solution of dipotassium phosphate on a rotary drum surface of a rotary drum scraper dryer which rotates continuously to form a material film with the thickness of 0.5 to 1.5mm, transferring heat to the material film on the rotary drum surface by using high-temperature heat-conducting oil as a heat transfer medium and heating the material film, scraping the rest material with a scraper after 92 to 97 percent of moisture is evaporated, and obtaining relatively humid granular or plate-like solid dipotassium phosphate with the moisture content of 3 to 8 percent; and continuously conveying the solid dipotassium phosphate into a rotary horizontal polymerization furnace to perform continuous dewatering and polymerization with reverse combustion gas or hot air generated by an air heater at the high temperature of 500 to 600 DEG C so as to generate potassium pyrophosphate, cooling, smashing, packaging and obtaining the potassium pyrophosphate products. The method can reduce the energy consumption of potassium pyrophosphate production; the production process is continuous and closed; environmental pollution is prevented; and the prepared potassium pyrophosphate has high content and high quality.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of method that adopts two-step approach continuous production potassium pyrophosphate.
Background technology
Potassium pyrophosphate is generally white powdery and clear crystal shape, very easily moisture absorption and deliquescence, anhydride molecular formula: K
4P
2O
7Be the fine chemical material product that is used for industries such as cyanideless electro-plating industry, food-processing industry, washing dyeing industry, ceramic industry, potassium pyrophosphate involved in the present invention is anhydride.The method of the potassium pyrophosphate of China's production at present mainly contains two kinds; One of which is " calcination method "; Promptly at first dipotassium hydrogen phosphate solution is concentrated and produce the potassium hydrogenphosphate crystal; Send in the calcining furnace further heat again and slough crystal water and molecular water, obtain the potassium pyrophosphate product 500-600 ℃ of following polymerization.This working method advantage is little for investment, and equipment is simple.Its shortcoming is that the mode of production is an intermittent type; Industrial scale is little, and production efficiency is low, because of material in the heated polymerizable process of potassium hydrogenphosphate is in static state; There is the bigger temperature difference in the material table; Thereby unstable product quality, according to the potassium pyrophosphate physics-chem characteristic of the moisture absorption very easily, also be difficult to accomplish clean environment firendly production.It two is " a horizontal polymerization furnace single stage method ", is about to dipotassium hydrogen phosphate solution and pressurizes with HPP, and through the atomizing of burner spray gun, with the combustion gas mixing of carrying out in the same way, the dehydration polymerisation step is accomplished, and obtains the potassium pyrophosphate product in horizontal polymerization furnace.This working system can be accomplished continuous production, and technical process is simple, but has two subject matters: the one, and type of heating adopts following current, and the polymerization temperature of product is 500-600 ℃, and the exhaust temperature of its tail gas reaches more than 500 ℃, causes heat energy to be wasted in a large number; The 2nd, the granular potassium hydrogenphosphate fine powder that produces in the atomization drying process, bulk density is less, for about 0.3-0.5g/cm3; Because of stopping the short potassium pyrophosphate that do not generate of polymerization time, a part causes unstable product quality to considerable potassium hydrogenphosphate particle suspension among the sedimentation of stove tail is brought into product in air-flow; Another part is brought into the washing tail gas system; A large amount of high-temperature vapors are mingled with dust discharges, and Dark smoke billows, has increased the pressure that environmental protection is produced.
Summary of the invention
Technical problem to be solved by this invention is: how a kind of method of two-step approach continuous production potassium pyrophosphate is provided, and this method can reduce the energy consumption that potassium pyrophosphate is produced significantly, and production process is sealed continuously, avoids environmental pollution; Higher, the stay in grade of potassium pyrophosphate content that adopts this method to produce.
Technical problem proposed by the invention is to solve like this: a kind of method of two-step approach continuous production potassium pyrophosphate is provided, it is characterized in that, comprise the steps:
Producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution;
Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 0.5-1.5mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to from the high temperature heat conductive oil of heat conducting oil boiler as heat-transfer medium the heating of constantly conducting heat of the material film of cylinder surface; To the moisture that evaporates 92-97%, scrape leftover materials, obtain water cut at the moistening relatively granular or flaky solid-state potassium hydrogenphosphate of 3-8% by scraper;
Producing of C, potassium pyrophosphate: this solid-state potassium hydrogenphosphate is sent in the horizontal polymerization furnace of rotation continuously; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration; Polymerization under 500-600 ℃ of temperature generates potassium pyrophosphate, obtains the potassium pyrophosphate finished product through the cooling crushing packing.
Method according to two-step approach continuous production potassium pyrophosphate provided by the present invention is characterized in that: in steps A, the proportion of control neutralizer is 1.5-1.8g/cm3, and pH value is 8.6-9.0.
Method according to two-step approach continuous production potassium pyrophosphate provided by the present invention is characterized in that: in step B, the temperature of thermal oil is 200 ℃-340 ℃.
Method according to two-step approach continuous production potassium pyrophosphate provided by the present invention is characterized in that: in step C, solid-state potassium hydrogenphosphate adopts spiral conveyer, belt conveyor or bucket elevator to send into continuously in the horizontal polymerization furnace of rotation.
Method according to two-step approach continuous production potassium pyrophosphate provided by the present invention is characterized in that: in step C, the potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace is taken away can obtain ADKP after being collected by tornado dust collector; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, in delivering to by blowback with recirculated water and in the still.
In sum, the method for two-step approach continuous production potassium pyrophosphate provided by the present invention has following advantage than prior art:
1, energy-saving and cost-reducing: the key equipment Rollingscratchboarddrier that the present invention adopts, its heat transfer theory are the consistent unidirectional heat transfers of direction from inside to outside, make heat-transfer medium with high temperature heat conductive oil, and dry tenacity is high, and thermo-efficiency can reach 80-90%.Granular or the sheet potassium hydrogenphosphate intermediates that make, water cut are at 3-8%, relatively weight in wet base; Can do not kicked up by hot blast, make countercurrent flow technology be able to successful implementation, the hot gas below 500 ℃ is used for preheating; The free-water of dephosphorylate hydrogen dipotassium and part molecular water; The exhaust emissions temperature is below 300 ℃, and heat energy is fully used, and thermo-efficiency is greatly improved.Compare with conventional fabrication processes, can save energy 40-60%.
2, high, the stay in grade of product content: because the dehydration polymerization process of article is in the polymerization furnace that constantly rotates, to carry out in the middle of the potassium hydrogenphosphate, material gets into from burner, and the stove wake flow goes out, and hot gas is then opposite.Material by upset constantly, has guaranteed that same cross section material temperature is in full accord therein, thereby has guaranteed the stable of product quality.In like manner, same cross section material temperature can be controlled at needed technological temperature than being easier to, thereby makes high-load product, and the content of product can reach more than 98%.After sending into cooling drum cooling from the effusive product of horizontal polymerization furnace afterbody, carry out crushing packing again.Whole technological process all is among the continuous closed state, makes quality product obtain strict guarantee.
3, production process clean environment firendly, pollution-free: the first step drying of this technology is a material film evaporation drying, and drying process has only moisture to be evaporated eliminating, and no material dust produces.In horizontal polymerization furnace, participate in polymeric material relative wet and big and heavy, be difficult for producing airborne dust, the powder of taking out of is on a small quantity collected by tornado dust collector, and the dust of trace is thoroughly washed by water wash column, thereby accomplishes clean environment firendly production.
4, succinct, the highly versatile of technical process: the temperature to this technology polymeric part adjusts slightly; Reduce to 200-300 ℃; Can make the good potassium hydrogenphosphate finished product of quality, overcome with spray-drying process and produced the shortcoming that energy consumption is high, yield is low that potassium hydrogenphosphate exists.Potassium phosphorus ratio to the neutralization part is adjusted, and can also make products such as potassium primary phosphate, Tripotassium phosphate, Potassium tripolyphosphate.Other are similar to the potassium pyrophosphate polymerization manufacturing of need dewatering has the phosphate product of corresponding characteristics, adopts this explained hereafter, all can benefit from the present invention's advantage.
Description of drawings
Fig. 1 is the process flow sheet of two-step approach continuous production potassium pyrophosphate provided by the present invention;
Fig. 2 produces the process flow sheet of ADKP for adopting method of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment of the present invention is carried out detailed description.
As shown in Figure 1, the method for two-step approach continuous production potassium pyrophosphate provided by the present invention comprises the steps: producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution; Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 0.5-1.5mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to from the high temperature heat conductive oil of heat conducting oil boiler as heat-transfer medium the heating of constantly conducting heat of the material film of cylinder surface; To the moisture that evaporates 92-97%, scrape leftover materials by scraper; Obtain water cut at the moistening relatively granular or flaky solid-state potassium hydrogenphosphate of 3-8%; Be convenient to carry out countercurrent flow, be unlikely to produce a large amount of airborne dusts at next step polymerization process and hot blast; Producing of C, potassium pyrophosphate: this solid-state potassium hydrogenphosphate is sent in the horizontal polymerization furnace of rotation continuously; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration, polymerization under 500-600 ℃ of high temperature, exhaust temperature 250-300 ℃; Generate potassium pyrophosphate, obtain the potassium pyrophosphate finished product through the cooling crushing packing.
In steps A, the proportion of control neutralizer is 1.5-1.8g/cm3, and pH value is 8.6-9.0.In step B, the temperature of thermal oil is 200 ℃-340 ℃.In step C, solid-state potassium hydrogenphosphate adopts spiral conveyer, belt conveyor or bucket elevator to send into continuously in the horizontal polymerization furnace of rotation; The potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace is taken away can obtain ADKP after being collected by tornado dust collector; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, utilize again in delivering to by blowback with recirculated water with in the still.
Embodiment 1:
Producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution, the proportion of control neutralizer is 1.5g/cm3, pH value is 9.0; Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 0.5mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to temperature from heat conducting oil boiler and be 200 ℃ thermal oil as heat-transfer medium to the heating of constantly conducting heat of the material film of cylinder surface; After evaporating 97% moisture, scrape leftover materials by scraper; Obtain water cut at 3% moistening relatively granular or flaky solid-state potassium hydrogenphosphate; Be convenient to carry out countercurrent flow, be unlikely to produce a large amount of airborne dusts at next step polymerization process and hot blast; Producing of C, potassium pyrophosphate: adopt spiral conveyer to send into continuously in the horizontal polymerization furnace of rotation this solid-state potassium hydrogenphosphate; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration, polymerization under 500 ℃ of temperature, 260 ℃ of exhaust temperatures; Generate potassium pyrophosphate, obtain the potassium pyrophosphate finished product through the cooling crushing packing; After simultaneously about 5% the potassium hydrogenphosphate pressed powder taken away of the tail gas of horizontal polymerization furnace is collected by tornado dust collector, can obtain ADKP; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, utilize again in delivering to by blowback with recirculated water with in the still.
Embodiment 2:
Producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution, the proportion of control neutralizer is 1.8g/cm3, pH value is 8.6; Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 1.5mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to temperature from heat conducting oil boiler and be 340 ℃ thermal oil as heat-transfer medium to the heating of constantly conducting heat of the material film of cylinder surface; After evaporating 92% moisture, scrape leftover materials by scraper; Obtain water cut at 8% moistening relatively granular or flaky solid-state potassium hydrogenphosphate; Be convenient to carry out countercurrent flow, be unlikely to produce a large amount of airborne dusts at next step polymerization process and hot blast; Producing of C, potassium pyrophosphate: adopt belt conveyor to send into continuously in the horizontal polymerization furnace of rotation this solid-state potassium hydrogenphosphate; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration, polymerization under 590 ℃ of temperature, 290 ℃ of exhaust temperatures; Generate potassium pyrophosphate, obtain the potassium pyrophosphate finished product through the cooling crushing packing; After the potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace of while is taken away is collected by tornado dust collector, can obtain ADKP; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, utilize again in delivering to by blowback with recirculated water with in the still.
Embodiment 3:
Producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution, the proportion of control neutralizer is 1.6g/cm3, pH value is 8.8; Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 1.0mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to temperature from heat conducting oil boiler and be 270 ℃ thermal oil as heat-transfer medium to the heating of constantly conducting heat of the material film of cylinder surface; After evaporating 95% moisture, scrape leftover materials by scraper; Obtain water cut at 5% moistening relatively granular or flaky solid-state potassium hydrogenphosphate; Be convenient to carry out countercurrent flow, be unlikely to produce a large amount of airborne dusts at next step polymerization process and hot blast; Producing of C, potassium pyrophosphate: adopt bucket elevator to send into continuously in the horizontal polymerization furnace of rotation this solid-state potassium hydrogenphosphate; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration, polymerization under 560 ℃ of temperature, 280 ℃ of exhaust temperatures; Generate potassium pyrophosphate, obtain the potassium pyrophosphate finished product through the cooling crushing packing; After the potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace of while is taken away is collected by tornado dust collector, can obtain ADKP; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, utilize again in delivering to by blowback with recirculated water with in the still.
As shown in Figure 2; The method of two-step approach continuous production potassium pyrophosphate provided by the present invention also can be used for continuous production ADKP solid; Concrete steps are following: the producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution; The proportion of control neutralizer is 1.5-1.8g/cm3, and pH value is 8.6-9.0; Being heating and curing of B, potassium hydrogenphosphate: dipotassium hydrogen phosphate solution sprayed to form thickness in the cylinder surface of the Rollingscratchboarddrier of continuous rotation be the material film of 0.5-1.5mm; Be used to temperature from heat conducting oil boiler and be 200-340 ℃ thermal oil as heat-transfer medium to the heating of constantly conducting heat of the material film of cylinder surface; To the moisture that evaporates 92-97%, scrape leftover materials, obtain water cut at the moistening relatively granular or flaky solid-state potassium hydrogenphosphate of 3-8% by scraper; Producing of C, ADKP: adopt spiral conveyer, belt conveyor or bucket elevator to send into continuously in the horizontal polymerization furnace of rotation this solid-state potassium hydrogenphosphate; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Under 200-300 ℃ of temperature, continue dehydration; Exhaust temperature is controlled at 100-150 ℃, obtains ADKP, obtains ADKP through the cooling crushing packing; After the potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace of while is taken away is collected by tornado dust collector, can obtain ADKP; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, utilize again in delivering to by blowback with recirculated water with in the still.
In sum, crucial drying plant of the present invention is a Rollingscratchboarddrier, and it is little to have floor space, and dry tenacity is high, advantages such as dry film-making granulation one step completion.The whole production system required drive is little, noiselessness, no dust, environmental protection and energy saving.Especially with traditional last charging with soak down the material mode and change linearity into and layout behind the spray, effective drying surface brings up to 96% from 75%, has improved thermo-efficiency, has guaranteed that simultaneously the product evenness of discharge stablizes.The full intelligent automatic control of heat conducting oil boiler heating system, SF is high.
Claims (5)
1. the method for a two-step approach continuous production potassium pyrophosphate is characterized in that, comprises the steps:
Producing of A, potassium hydrogenphosphate: with phosphoric acid and Pottasium Hydroxide in still in reaction obtain dipotassium hydrogen phosphate solution;
Being heating and curing of B, potassium hydrogenphosphate: it is the material film of 0.5-1.5mm that dipotassium hydrogen phosphate solution spray or the cylinder surface that soaks the Rollingscratchboarddrier that invests continuous rotation are formed thickness; Be used to from the high temperature heat conductive oil of heat conducting oil boiler as heat-transfer medium the heating of constantly conducting heat of the material film of cylinder surface; To the moisture that evaporates 92-97%, scrape leftover materials, obtain water cut at the moistening relatively granular or flaky solid-state potassium hydrogenphosphate of 3-8% by scraper;
Producing of C, potassium pyrophosphate: this solid-state potassium hydrogenphosphate is sent in the horizontal polymerization furnace of rotation continuously; Carry out countercurrent flow with the burning gas or the warm air that produce by hotblast stove; Continue dehydration; Polymerization under 500-600 ℃ of temperature generates potassium pyrophosphate, obtains the potassium pyrophosphate finished product through the cooling crushing packing.
2. the method for two-step approach continuous production potassium pyrophosphate according to claim 1 is characterized in that: in steps A, the proportion of control neutralizer is 1.5-1.8g/cm
3, the pH value is 8.6-9.0.
3. the method for two-step approach continuous production potassium pyrophosphate according to claim 1 is characterized in that: in step B, the temperature of thermal oil is 200 ℃-340 ℃.
4. the method for two-step approach continuous production potassium pyrophosphate according to claim 1 is characterized in that: in step C, solid-state potassium hydrogenphosphate adopts spiral conveyer, belt conveyor or bucket elevator to send into continuously in the horizontal polymerization furnace of rotation.
5. according to the method for claim 1 or 4 described two-step approach continuous production potassium pyrophosphates; It is characterized in that: in step C; The potassium hydrogenphosphate pressed powder that the tail gas of horizontal polymerization furnace is taken away can obtain ADKP after being collected by tornado dust collector; Thoroughly wash remaining potassium hydrogenphosphate pressed powder by water wash column recirculated water more afterwards, in delivering to by blowback with recirculated water and in the still.
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| CN102538199B (en) * | 2011-12-29 | 2014-12-17 | 广西利达磷化工有限公司 | Method for absorbing and recycling yellow phosphorus burning heat by using heat-conducting oil |
| CN105967165B (en) * | 2016-07-04 | 2018-12-14 | 湖北兴发化工集团股份有限公司 | A kind of production process and device that grade potassium pyrophosphate is electroplated |
| CN110371942B (en) * | 2019-08-01 | 2023-05-09 | 四川金地亚美科技有限公司 | Production process of heavy potassium pyrophosphate returning flow |
| CN110482510A (en) * | 2019-09-20 | 2019-11-22 | 瓮福达州化工有限责任公司 | A kind of preparation process of food grade phosphoric acid hydrogen dipotassium |
| CN112062116A (en) * | 2020-08-26 | 2020-12-11 | 华融化学股份有限公司 | Potassium pyrophosphate continuous production line, production method and production control system |
| 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 |
| CN113816355B (en) * | 2021-11-08 | 2023-08-22 | 云南云天化股份有限公司 | Method and device for preparing potassium pyrophosphate and co-producing water-soluble fertilizer through one-step dehydration polymerization |
| CN113942989A (en) * | 2021-11-30 | 2022-01-18 | 泰山石膏有限公司 | Device and method for continuously producing sodium trimetaphosphate by two-step method |
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| GB939318A (en) * | 1959-12-23 | 1963-10-09 | Stauffer Chemical Co | Method for the manufacture of alkali metal polyphosphate compositions |
| CN101723342B (en) * | 2009-10-28 | 2011-05-18 | 广东光华科技股份有限公司 | Method for preparing electronic grade high-purity potassium permanganate |
| CN101708836B (en) * | 2009-12-11 | 2012-09-05 | 宜昌楚磷化工有限公司 | Method for preparing disodium dihydrogen pyrophosphate by adopting dynamic polymerization furnace |
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