CN107715549A - A kind of potassium fluosilicate/sodium separation device and its application - Google Patents

A kind of potassium fluosilicate/sodium separation device and its application Download PDF

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Publication number
CN107715549A
CN107715549A CN201710804597.9A CN201710804597A CN107715549A CN 107715549 A CN107715549 A CN 107715549A CN 201710804597 A CN201710804597 A CN 201710804597A CN 107715549 A CN107715549 A CN 107715549A
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China
Prior art keywords
separation device
potassium fluosilicate
sodium separation
sodium
outlet
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CN201710804597.9A
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CN107715549B (en
Inventor
邓信立
杨业信
张俊
黄玲贵
吴敏军
范宁
严勇
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Chemical Industry Co Ltd Of Wengfu Dazhou City
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Chemical Industry Co Ltd Of Wengfu Dazhou City
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D33/00Filters with filtering elements which move during the filtering operation
    • B01D33/01Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons
    • B01D33/03Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons with vibrating filter elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/04Combinations of filters with settling tanks
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/18Phosphoric acid
    • C01B25/22Preparation by reacting phosphate-containing material with an acid, e.g. wet process
    • C01B25/222Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
    • C01B25/223Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
    • C01B25/225Dihydrate process

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of potassium fluosilicate/sodium separation device and its application, the separator is arranged on the bottom for dodging cold return pipe, it includes a separating pipe, the separating pipe includes inducer and outlet section, gate valve is installed between inducer and outlet section, the exit of outlet section is provided with gate valve, and screening plant is provided with outside the outlet of separating pipe outlet section, spray equipment is provided between the screening plant and the outlet of separating pipe.Potassium fluosilicate/sodium separation device provided by the invention is simple in construction, it is easy to use, the bottom of cold return pipe is dodged by being installed in, effectively potassium fluosilicate/sodium foulant is separated from reaction slurry, avoid the k-na salt foulant to endanger to caused by reactive tank and pipeline, improve production efficiency.

Description

A kind of potassium fluosilicate/sodium separation device and its application
Technical field
The present invention relates to a kind of separator and its application, and in particular to a kind of potassium fluosilicate/sodium separation device and its should With belonging to Wet-process Phosphoric Acid Production equipment technical field.
Background technology
Phosphoric acid is the production technology master of the basic material for producing various industry and agricultural phosphorus product, at present domestic and international phosphoric acid Have two kinds of Re Fa and wet method, the two compares, and the process characteristic of phosphoric acid by wet process is that product cost is relatively low, but quality compared with Difference.Preparing industrial phosphoric acid in the world mainly uses wet method at present, and China's phosphoric acid by wet process is mainly for the production of agricultural chemical fertilizer.It is so-called Phosphoric acid by wet process, it is to use inorganic acid decomposing rock phosphate with hydrogen, raw phosphoric acid, then purified rear obtained phosphoric acid product is isolated, wherein accounting for leading Status is sulfuric acid process phosphoric acid by wet process, and ore decomposition reaction equation is:
Ca5F(PO4)3+5H2SO4+nH2O=3H3PO4+5CaSO4·nH2O+HF↑
Wherein n value depends on the form of crystal of calcium sulfate, can be 0,1/2,2.In different reaction temperature and phosphoric acid Under concentration, dead plaster, half-H 2 O calcium sulphate and calcium sulphate dihydrate can be generated.At present, the phosphoric acid in China more than 80% is all adopted Produced with the water law flow of phosphoric acid by wet process two.
Using high potassium, sodium content phosphorus ore as in the Wet-process Phosphoric Acid Production of raw material, the fluorine of band is by reaction generation fluorine in ore pulp Silicic acid, then it is incorporated in formation potassium fluosilicate/sodium saturated solution, chemical formula R in reactive tank with the potassium in phosphorus ore, sodium impurity2SiF6 (R K, Na), is white particle or crystalline powder, and high temperature (more than 300 DEG C) is decomposed into RF and SiF4.Show as crystallizing when a small amount of Powder, pipeline and inner surface of container are attached to, the time one, which is grown, easily blocks pipeline, influences to generate load;Shown as when a large amount of It is granular, settled down in reactive tank and be difficult to separate, directly affect reactive tank dischargeable capacity, reduce stirring intensity, had greatly Hidden danger.When acidolysis slurry filtration separates, because vacuum action makes moisture drastically vaporize, temperature decrease is filtering up to 25~30 DEG C Pipe-line system will separate out potassium fluosilicate/sodium dirt layer of hard and compact, block pipeline, influence produce load, this turned into high potassium, The main technique problem of sodium content phosphorus ore Wet-process Phosphoric Acid Production.
The content of the invention
In view of this, in view of the shortcomings of the prior art, the present invention provides a kind of potassium fluosilicate/sodium separation device and its should With to solve the problems, such as to be previously mentioned in above-mentioned background technology.
To solve above technical problem, the technical scheme is that using a kind of potassium fluosilicate/sodium separation device, it is wrapped A separating pipe is included, the separating pipe includes inducer and outlet section, gate valve, outlet section are provided between inducer and outlet section Exit gate valve is installed, be provided with screening plant outside the outlet of separating pipe outlet section, the screening plant and separating pipe Spray equipment is provided between outlet.
Further, in addition to a source of the gas supplies control system, and the gate valve is Pneumatic gate valve, supplies and controls with source of the gas System connects.
Preferably, the gate valve installed between the separating pipe inducer and outlet section is pneumatic knife gate valve.
Preferably, the gate valve of the exit installation of the separating pipe outlet section presss from both sides valve for gas.
Preferably, the screening plant is vibratory sieve.
Preferably, a diameter of 500mm of the inducer, length 500mm, a diameter of 150mm of outlet section, length For 5000mm.
Preferably, it is tapered buffering connection between the inducer and outlet section, tapered height is 250mm.
Meanwhile present invention also offers the application process of above-mentioned potassium fluosilicate/sodium separation device, it is by above-mentioned fluorine silicon Sour potassium/sodium separation device is arranged on the bottom for dodging cold return pipe.
Preferably, the bottom for dodging cold return pipe is at least spaced and is provided with two above-mentioned potassium fluosilicate/sodium separation devices.
Further, the absolute pressure for keeping dodging cold return pipe is -40KPa.
In dihydrate wet-process phosphoric acid production technology, the reaction temperature of phosphorus ore, sulfuric acid and phosphoric acid in reactive tank should maintain 75~80 DEG C, reaction could generate two water thing calcium sulfate (CaS04·2H2O) crystallization and phosphoric acid.Phosphate ore pulp is through metering and and raw material The first Room of rectangle reactive tank is added after sulfuric acid regulation ratio, rectangle reactive tank is made up of the Room of identical six, had three layers per the equal band in room The agitator of blade.Because heat caused by sulfuric acid dilution and exothermic reaction can raise reaction slurry temperature, in order to react For temperature control at 75~80 DEG C, guarantee obtains two water thing crystal of calcium sulfate, it is necessary to which reaction slurry is cooled down.
Flash principle is widely used in dihydrate wet phosphoric acid generation, and effect is exactly to remove the amount of heat of reaction generation, it Reaction slurry is got to by flash chamber from six Room of reaction by axial-flow pump, under suction function, gas phase takes away amount of heat after flash distillation, Reaction slurry then returns to one Room of reaction, so circulation by dodging cold return pipe.Potassium fluosilicate/sodium separation device of the present invention just designs Dodging cold return pipe position.Through measuring and calculating, the proportion of potassium fluosilicate/sodium foulant is generally in more than 2.6g/mL, the phase of reaction slurry 1.6g/mL is typically not greater than to density, using this difference in specific gravity, (keeps absolute pressure 40kPa) under the suction function of return pipe, proportion Big potassium fluosilicate/sodium foulant is preferentially settled into the separating pipe being connected with dodging cold return pipe, and reaction slurry is then cold with dodging Return pipe returns to reactive tank;The slurry carried secretly in potassium fluosilicate/sodium foulant is separated by filtration by spray equipment washing, vibratory sieve After reclaim;The k-na salt finally obtained i.e. potassium fluosilicate/sodium foulant is directly transferred out of system.In the process, source of the gas is supplied Control system presss from both sides the opening and closing of valve according to the pneumatic knife gate valve of how much automatic control and adjustments of k-na salt amount with gas, it is possible to achieve above opens down Close, under the effect shut out, rationally control the back amount of reaction slurry, ensure normal production.
Compared with prior art, potassium fluosilicate/sodium separation device provided by the invention is simple in construction, easy to use, passes through The bottom for dodging cold return pipe is installed in, effectively potassium fluosilicate/sodium foulant is separated from reaction slurry, avoided The k-na salt foulant endangers to caused by reactive tank and pipeline, improves production efficiency.
Brief description of the drawings
Fig. 1 is the structural representation of potassium fluosilicate/sodium separation device of the present invention;
Fig. 2 is the scheme of installation of potassium fluosilicate/sodium separation device of the present invention.
Marginal data:
1- reactive tanks, 2- axial-flow pumps, 3- dodge cold vaporization chamber, and 4- dodges cold return pipe, 5- potassium fluosilicates/sodium separation device;
The Room of 11- reactive tanks six, the Room of 12- reactive tanks one;
51- separating pipes, the pneumatic knife gate valves of 52-, 53- gas folder valve, 54- spray equipments, 55- vibratory sieves;
511- inducers, 512- outlet sections.
Embodiment
In order that those skilled in the art more fully understands technical scheme, it is below in conjunction with the accompanying drawings and preferred real Applying mode, the present invention is described in further detail.It should be pointed out that following preferred embodiments are not construed as to this hair Bright limitation, protection scope of the present invention should be defined by claim limited range.For the common of the art For technical staff, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these improve and Retouching also should be regarded as protection scope of the present invention.
Referring to Fig. 1, the invention provides a kind of potassium fluosilicate/sodium separation device, it includes a separating pipe 51, described point Include inducer 511 and outlet section 512 from pipe, pneumatic knife gate valve 52 is installed between inducer 511 and outlet section 512, export The exit of section is provided with gas folder valve 53, and small-size vibration screen 55, the vibratory sieve are provided with outside the outlet of separating pipe outlet section 512 Spray equipment 54 is provided between 55 and the outlet of separating pipe 51.Also include a source of the gas simultaneously and supply control system, pneumatic knife Gate valve 52 is connected with source of the gas supply control system respectively with gas folder valve 53.
Preferably, a diameter of 500mm of the inducer 511, length 500mm, outlet section 512 it is a diameter of 150mm, length 5000mm.
Preferably, it is that tapered buffering connects between the inducer 511 and outlet section 512, tapered height is 250mm。
Referring to Fig. 2, the application process of potassium fluosilicate/sodium separation device provided by the invention is by the potassium fluosilicate/sodium point The bottom for dodging cold return pipe 4 is arranged on from device 5.
Preferably, the bottom for dodging cold return pipe is at least spaced and is provided with two above-mentioned potassium fluosilicate/sodium separation devices.
Further, the absolute pressure for keeping dodging cold return pipe is -40KPa.
Referring to Fig. 2, axial-flow pump 2, which gets to reaction slurry from the Room 11 of reactive tank six, dodges cold vaporization chamber 3, under suction function, Gas phase takes away amount of heat after flash distillation, and reaction slurry then returns to the Room 12 of reactive tank one, so circulation by dodging cold return pipe 4.This Invention potassium fluosilicate/sodium separation device 5 is just arranged on the bottom for dodging cold return pipe 4.Through calculating, potassium fluosilicate/sodium foulant Proportion is generally typically not greater than 1.6g/mL in more than 2.6g/mL, the relative density of reaction slurry, cold dodging using this difference in specific gravity (absolute pressure 40kPa is kept under the suction function of return pipe), and heavy potassium fluosilicate/sodium foulant preferentially settles into cold with sudden strain of a muscle In the separating pipe 51 of return pipe connection, reaction slurry then returns to reactive tank 1 with the cold return pipe 4 of sudden strain of a muscle;In potassium fluosilicate/sodium foulant The slurry of entrainment reclaims after spray equipment 54 is washed, vibratory sieve 55 is separated by filtration;The k-na salt finally obtained i.e. fluosilicic acid Potassium/sodium foulant is directly transferred out of system.In the process, source of the gas supply control system is controlled automatically according to the how much of k-na salt amount System adjusts the opening and closing of pneumatic knife gate valve 52 and gas folder valve 53, it is possible to achieve above open ShiShimonoseki, under the effect shut out, rationally control is anti- The back amount of slurry is answered, ensures normal production.
Pass through the reality on the dihydrate wet-process phosphoric acid production line of chemical industry Co., Ltd of the applicant's Wengfu Dazhou City Using showing, the production line of separator of the present invention is mounted with, the equipment and pipeline cleaning of its filter progress and enrichment process 1.5 times of cycle stretch-out, clearance time also shorten to original 30~35%, substantially increase production efficiency.

Claims (10)

  1. A kind of 1. potassium fluosilicate/sodium separation device, it is characterised in that:Including a separating pipe, the separating pipe includes inducer With outlet section, gate valve is installed between inducer and outlet section, the exit of outlet section is provided with gate valve, separating pipe outlet section Outlet is outer to be provided with screening plant, and spray equipment is provided between the screening plant and the outlet of separating pipe.
  2. A kind of 2. potassium fluosilicate/sodium separation device according to claim 1, it is characterised in that:Also include a source of the gas to supply Control system is answered, the gate valve is Pneumatic gate valve, is connected with source of the gas supply control system.
  3. A kind of 3. potassium fluosilicate/sodium separation device according to claim 1 or 2, it is characterised in that:The separating pipe import The gate valve installed between section and outlet section is pneumatic knife gate valve.
  4. A kind of 4. potassium fluosilicate/sodium separation device according to claim 1 or 2, it is characterised in that:The separating pipe outlet The gate valve of the exit installation of section presss from both sides valve for gas.
  5. A kind of 5. potassium fluosilicate/sodium separation device according to claim 1, it is characterised in that:The screening plant is to shake Dynamic sieve.
  6. A kind of 6. potassium fluosilicate/sodium separation device according to claim 1, it is characterised in that:The diameter of the inducer For 500mm, length 500mm, a diameter of 150mm of outlet section, length 5000mm.
  7. A kind of 7. potassium fluosilicate/sodium separation device according to claim 1, it is characterised in that:The inducer and outlet It is tapered buffering connection between section, tapered height is 250mm.
  8. A kind of 8. application of potassium fluosilicate/sodium separation device, it is characterised in that:By the fluorine any one of claim 1-7 Potassium silicate/sodium separation device is arranged on the bottom for dodging cold return pipe.
  9. A kind of 9. application of potassium fluosilicate/sodium separation device according to claim 8, it is characterised in that:It is described to dodge cold time The bottom of slurry pipe is at least spaced the potassium fluosilicate/sodium separation device being provided with any one of two claim 1-7.
  10. A kind of 10. application of potassium fluosilicate/sodium separation device according to claim 8 or claim 9, it is characterised in that:Keep dodging The absolute pressure of cold return pipe is -40KPa.
CN201710804597.9A 2017-09-08 2017-09-08 Potassium fluosilicate/sodium fluosilicate separation device and application thereof Active CN107715549B (en)

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Application Number Priority Date Filing Date Title
CN201710804597.9A CN107715549B (en) 2017-09-08 2017-09-08 Potassium fluosilicate/sodium fluosilicate separation device and application thereof

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5891021A (en) * 1981-11-27 1983-05-30 Toyo Soda Mfg Co Ltd Manufacture of wet process phosphoric acid
CN102380233A (en) * 2011-09-21 2012-03-21 云南大红山管道有限公司 Dewatering treatment device for low-concentration pulp in pipes and treatment method of dewatering treatment device
CN102390821A (en) * 2011-08-08 2012-03-28 云南云天化国际化工股份有限公司 Method for producing dihydrate wet-process phosphoric acid
CN202212352U (en) * 2011-08-22 2012-05-09 山东昌邑石化有限公司 Balancing agent filter
CN202263430U (en) * 2011-09-21 2012-06-06 云南大红山管道有限公司 Dehydrating treatment device for low-concentration slurry in pipeline
CN202643330U (en) * 2012-06-28 2013-01-02 贵州开磷(集团)有限责任公司 Device for preparing high-purity ammonium fluosilicate
CN105776221A (en) * 2016-04-01 2016-07-20 龚家竹 Method for recycling fluorine resources in phosphate fertilizer production

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5891021A (en) * 1981-11-27 1983-05-30 Toyo Soda Mfg Co Ltd Manufacture of wet process phosphoric acid
CN102390821A (en) * 2011-08-08 2012-03-28 云南云天化国际化工股份有限公司 Method for producing dihydrate wet-process phosphoric acid
CN202212352U (en) * 2011-08-22 2012-05-09 山东昌邑石化有限公司 Balancing agent filter
CN102380233A (en) * 2011-09-21 2012-03-21 云南大红山管道有限公司 Dewatering treatment device for low-concentration pulp in pipes and treatment method of dewatering treatment device
CN202263430U (en) * 2011-09-21 2012-06-06 云南大红山管道有限公司 Dehydrating treatment device for low-concentration slurry in pipeline
CN202643330U (en) * 2012-06-28 2013-01-02 贵州开磷(集团)有限责任公司 Device for preparing high-purity ammonium fluosilicate
CN105776221A (en) * 2016-04-01 2016-07-20 龚家竹 Method for recycling fluorine resources in phosphate fertilizer production

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