CN106809811B - A method of sodium pyrophosphate is prepared using crude product sodium pyrophosphate - Google Patents

A method of sodium pyrophosphate is prepared using crude product sodium pyrophosphate Download PDF

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CN106809811B
CN106809811B CN201710150364.1A CN201710150364A CN106809811B CN 106809811 B CN106809811 B CN 106809811B CN 201710150364 A CN201710150364 A CN 201710150364A CN 106809811 B CN106809811 B CN 106809811B
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sodium pyrophosphate
mother liquor
crude product
sodium
filtrate
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CN106809811A (en
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詹波
朱建民
姜胜宝
刘冰
张立新
郑新
王垚
魏利
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ZHENJIANG JIANGNAN CHEMICAL CO Ltd
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ZHENJIANG JIANGNAN CHEMICAL CO Ltd
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    • 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
    • C01B25/26Phosphates
    • C01B25/38Condensed phosphates
    • C01B25/42Pyrophosphates
    • C01B25/425Pyrophosphates of alkali metals

Abstract

The present invention relates to a kind of methods for preparing sodium pyrophosphate using crude product sodium pyrophosphate, the steps include: (1) crude product sodium pyrophosphate washing mashing: 1. previous cleaning;2. filtering;3. being beaten;(2) sodium pyrophosphate purifies: after diluted sodium pyrophosphate slurries and molten slag filtrate mixed dissolution, addition activated carbon adsorption, carry out secondary filter, obtain secondary filter filtrate and secondary filter filter residue, by secondary filter filtrate crystallisation by cooling, it can be obtained after filtering and apply sodium pyrophosphate mother liquor and sodium pyrophosphate;(3) cycling and reutilization of sodium pyrophosphate mother liquor, sodium pyrophosphate disposing mother liquor is utilized, it is applied to washing and the solvent of crude product sodium pyrophosphate simultaneously, the yield of sodium pyrophosphate greatly improved, reduce the content of sodium pyrophosphate in slag charge, business efficiency is improved, efficiency has been saved, is reduced costs.

Description

A method of sodium pyrophosphate is prepared using crude product sodium pyrophosphate
Technical field
The present invention relates to a kind of Sodium pyrophosphate preparation technology fields, and in particular to a kind of to prepare coke using crude product sodium pyrophosphate The method of sodium phosphate.
Background technique
Sodium pyrophosphate is an important species in condensed phosphate.Either technical grade and food-grade, dosage are only secondary In sodium tripolyphosphate.Industrially it is mainly used for complexing agent, degreasing agent, water treatment agent, washing printing and dyeing bleaching assistant, dispersing agent etc.. Water holding in food industry then for food is fresh-keeping, anti-oxidant etc., is referred to as quality improver.With China's technical grade and food The market of grade sodium pyrophosphate is grown rapidly, and associated core production technology application is researched and developed to become with improvement and be looked forward in the industry The concern of industry.The improvement of the production technology of sodium pyrophosphate and research and development are very crucial for enterprise's promotion market competitiveness.And burnt phosphorus Sour sodium demand is just in the trend that increases substantially year by year.According to statistics, national sodium pyrophosphate volume of production and marketing annual average rate of increase is 7% or so, so the development potentiality in pyrophosphoric acid market is very big.
Crude product sodium pyrophosphate is that phosphorus-containing wastewater is obtained in high temperature furnace by flame incineration at present, due in burning process Local temperature it is higher, keep reaction uneven, be also easy to produce that hardness is higher and micro- waste residue material of agglomeration, this part slag charge is difficult molten Solution, and the content of sodium pyrophosphate reaches 40-70wt% in slag charge, causes the wasting of resources.
Summary of the invention
The present invention proposes a kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate regarding to the issue above, by burnt phosphorus Sour mother liquid of sodium recycles, while being applied to washing and the solvent of crude product sodium pyrophosphate, and the yield of sodium pyrophosphate greatly improved, The content for reducing sodium pyrophosphate in slag charge, improves business efficiency, has saved efficiency, reduces costs.
Specific technical solution is as follows:
A method of sodium pyrophosphate being prepared using crude product sodium pyrophosphate, the steps include:
(1) crude product sodium pyrophosphate washing mashing:
1. previous cleaning: crude product sodium pyrophosphate and sodium pyrophosphate mother liquor being added in the stirred tank with filter plate, at 0-30 DEG C At a temperature of stir 0.5-4h so that hydration reaction occurs for the water in anhydrous sodium pyrophosphate and sodium pyrophosphate mother liquor, form the crystallization water Close object, recycle sodium pyrophosphate mother liquor in part water, while in crude product sodium chloride and organic matter wash, enter surplus In remaining sodium pyrophosphate mother liquor, the purpose of concentrate sodium pyrophosphate mother liquor is played, and removes reaction heat in its reaction process or incites somebody to action Sodium pyrophosphate mother liquor is previously cooled to 15 DEG C or less and is washed again, finally obtains mixed liquor;
2. filtering: after mixed liquor is reacted in a stirring kettle and washed completely, extracting or extrude 50%- out by filter plate 80% filtrate, the filtrate for retaining 20-50% in slurry, avoid solid block in kettle, maintain stirring;
3. mashing discharging: be added immediately into stirred tank after filtering heat sodium pyrophosphate apply mother liquor re-start beat Slurry, so that sodium pyrophosphate dissolution of crystals, obtains diluted sodium pyrophosphate slurries after mixing evenly;
(2) sodium pyrophosphate purifies:
Diluted sodium pyrophosphate slurries and molten slag filtrate are mixed, oxidant is added after completely dissolution, progress oxidation reaction, And activated carbon adsorption oily organic matter and Fe is added by after pH value adjustment to 11-12 using sodium hydroxide solution3+The colloid of formation Precipitating carries out secondary filter, obtains secondary filter filtrate and secondary filter filter residue, by hydrochloric acid or phosphoric acid by secondary filter filtrate PH value adjustment to 9.8-10.5 after, by secondary filter filtrate crystallisation by cooling, can be obtained after filtering and apply sodium pyrophosphate mother liquor And sodium pyrophosphate;
(3) cycling and reutilization of sodium pyrophosphate mother liquor:
Apply sodium pyrophosphate mother liquor according to 1:(1-4 for what is be obtained by filtration in step (2)) volume ratio be divided into and apply burnt phosphorus Sour mother liquid of sodium (1) and apply sodium pyrophosphate mother liquor (2), apply sodium pyrophosphate mother liquor (1) alternative steps (1) 1. in sodium pyrophosphate Mother liquor, apply sodium pyrophosphate mother liquor (2) for step (1) 3. in be beaten.
A kind of above-mentioned method for preparing sodium pyrophosphate using crude product sodium pyrophosphate, wherein the active carbon accounts for crude product coke phosphorus The 0.02-0.1wt% of sour sodium slurries, active carbon and molten slag filtrate mixed liquor.
A kind of above-mentioned method for preparing sodium pyrophosphate using crude product sodium pyrophosphate, wherein the preparation side of the molten slag filtrate Method are as follows: by secondary filter filter residue and 80-100 DEG C of water in bubbling or strong mixing, obtain solid waste and molten slag after carrying out filters pressing Filtrate.
A kind of above-mentioned method for preparing sodium pyrophosphate using crude product sodium pyrophosphate, wherein the oxidant is hydrogen peroxide, chlorine Sour sodium, chlorine dioxide, combination one or more in ozone.
A kind of above-mentioned method for preparing sodium pyrophosphate using crude product sodium pyrophosphate, wherein washing dress is used in step (1) It sets, the wash mill includes stirred tank, waste tank and dissolution kettle, and paddle, paddle lower section are equipped in the stirred tank Equipped with filter plate, filter plate will be separated into stirred tank stir chamber and filter chamber, stirred tank be equipped with first charging aperture, second into Material mouth, suction filtration mouth and discharge port, first charging aperture and second charging aperture are located at the top of stirred tank, are connected with stir chamber, take out Filter mouth is located at the bottom of stirred tank, is connected with chamber is filtered, discharge port is between first charging aperture and suction filtration mouth, with stir chamber It is connected;Suction filtration mouth is connected by first pipe with the third feed inlet of waste tank, discharge port by second pipe with it is molten Solution kettle is connected.
The invention has the benefit that
(1) fresh water consumption and sodium pyrophosphate mother liquor amount to be treated is greatly lowered in the present invention;Raw material is reduced to bring into The impurity (sodium chloride and organic matter that can remove 50-80% in crude product) of production reduces production difficulty and production cost, improves and produces Quality;
The characteristics of present invention is saturated using low temperature mother liquor coke sodium washs sodium pyrophosphate crude product, avoids the damage of utility Lose, and by crude product partial oxidation sodium and a small amount of organic matter remove, reduce the impurity that raw band enters in burnt sodium purification production, make Production is more easier, and product quality is more preferable, and mother liquid recycle number is more;
The characteristic that the crystallization water is formed using the moisture in anhydrous sodium pyrophosphate absorption mother liquor in sodium pyrophosphate crude product, by mother liquor In moisture absorption, can use dissolution process in solid form, reduce industrial water amount, save final sodium pyrophosphate mother liquor amount And processing cost;
The 50-80wt% of the filtrate of extraction, makes residual filtrate not agglomerate, and is conducive to subsequent processing, makes filtrate distribution more Uniformly, subsequent processing is not easy to be blocked.
(2) present invention is handled using oxidant, is kept away during crude product sodium pyrophosphate purifies production sodium pyrophosphate and produces Exempting from the precipitations such as other microsolubility phosphoric acid (pyrophosphoric acid) aluminium salts, phosphoric acid (pyrophosphoric acid) molysite, phosphoric acid (pyrophosphoric acid) calcium salt influences product Quality, solve that sodium pyrophosphate product is rubescent or product storage and use in rubescent problem;It reduces impurity phosphoric acid (pyrophosphoric acid) Salt brings sodium pyrophosphate product into, influences crystal habit, improves product quality, solves the problems, such as the production of filtration difficulty.
(3) mother liquor is reused by applying a large amount of unsaturated mother liquors, reduces final mother liquor amount by the present invention;Greatly Width improves the yield of sodium pyrophosphate, reduces the content of sodium pyrophosphate in slag charge, improves business efficiency, has saved efficiency, It reduces costs;
The present invention avoids in material slightly soluble impurity to melting by the Special use method of sodium pyrophosphate mother liquor and water The dissolution of object influences, and significantly improves solution rate and dissolution degree, is greatly lowered and abandons solid waste amount;Impurity in solid waste is sandwiched Sodium pyrophosphate is returned, and the yield 10-30% of burnt sodium product is improved.
(4) present invention cooperation wash mill uses, and first filters portion filtrate in washing process, and filter residue is made to be in sticky but not The state being fully cured adds the new direct rising temperature for dissolving of sodium pyrophosphate mother liquor, then move into dissolution kettle carry out in next step it is anti- It answers, simplifies process, improve efficiency, reduce costs.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is wash mill cross-sectional view of the present invention.
Fig. 3 is filter plate cross-sectional view of the present invention.
Fig. 4 is sheet frame cross-sectional view of the present invention.
Fig. 5 is present invention filtering board group explosive view.
Fig. 6 is filter plate top view of the present invention.
Specific embodiment
It is clear to be more clear technical solution of the present invention, below the present invention is described further, any pair of sheet The technical characteristic of inventive technique scheme carries out the scheme that equivalencing is obtained with conventional reasoning and each falls within the scope of the present invention.
Embodiment one
A kind of wash mill for the washing mashing of crude product sodium pyrophosphate, including stirred tank 1, waste tank 2 and dissolution kettle 3, the stirred tank is interior to be equipped with paddle 4, is equipped with filter plate 5 below paddle, filter plate will be separated into stir chamber 6 in stirred tank With filter chamber 7, stirred tank be equipped with first charging aperture 8, second charging aperture 9, suction filtration mouth 10 and discharge port 11, first charging aperture and Second charging aperture is located at the top of stirred tank, is connected with stir chamber, and suction filtration mouth is located at the bottom of stirred tank, is connected with chamber is filtered Logical, discharge port is connected between first charging aperture and suction filtration mouth with stir chamber;Suction filtration mouth passes through first pipe 12 and waste liquid The third feed inlet of storage tank is connected, and discharge port is connected by second pipe 13 with dissolution kettle.
A method of sodium pyrophosphate being prepared using crude product sodium pyrophosphate, its step are as follows:
(1) crude product sodium pyrophosphate washing mashing:
1. previous cleaning: crude product sodium pyrophosphate and sodium pyrophosphate mother liquor being added in the stirred tank with filter plate, in 22 DEG C of temperature Degree is lower to stir 3h, so that hydration reaction occurs for the water in anhydrous sodium pyrophosphate and sodium pyrophosphate mother liquor, forms crystalline hydrate, returns Receive the part water in sodium pyrophosphate mother liquor, at the same in crude product sodium chloride and organic matter wash, enter remaining burnt phosphorus In sour mother liquid of sodium, the purpose of concentrate sodium pyrophosphate mother liquor is played, and removes in its reaction process reaction heat or by pyrophosphoric acid Mother liquid of sodium is previously cooled to 15 DEG C or less and is washed again, finally obtains mixed liquor;
2. filtering: after mixed liquor is reacted in a stirring kettle and washed completely, extracting or extrude 72% out by filter plate Filtrate, the filtrate for retaining 28% in slurry, avoid solid block in kettle, maintain stirring;
3. mashing discharging: be added immediately into stirred tank after filtering heat sodium pyrophosphate apply mother liquor re-start beat Slurry, so that sodium pyrophosphate dissolution of crystals, obtains diluted sodium pyrophosphate slurries after mixing evenly;
(2) sodium pyrophosphate purifies:
Diluted sodium pyrophosphate slurries and molten slag filtrate are mixed, oxidant is added after completely dissolution, progress oxidation reaction, And activated carbon adsorption oily organic matter and Fe is added by after pH value adjustment to 12 using sodium hydroxide solution3+The colloid of formation is heavy It forms sediment, carries out secondary filter, obtain secondary filter filtrate and secondary filter filter residue, by hydrochloric acid or phosphoric acid by secondary filter filtrate PH value adjustment, by secondary filter filtrate crystallisation by cooling, can be obtained after filtering to after 10 and apply sodium pyrophosphate mother liquor and pyrophosphoric acid Sodium;
(3) cycling and reutilization of sodium pyrophosphate mother liquor:
The sodium pyrophosphate mother liquor of applying being obtained by filtration in step (2) is divided into according to the volume ratio of 1:1.5 and applies pyrophosphoric acid Mother liquid of sodium (1) and apply sodium pyrophosphate mother liquor (2), apply sodium pyrophosphate mother liquor (1) alternative steps (1) 1. in sodium pyrophosphate it is female Liquid, apply sodium pyrophosphate mother liquor (2) for step (1) 3. in be beaten.
The active carbon accounts for the 0.05wt% of crude product sodium pyrophosphate slurries, active carbon and molten slag filtrate mixed liquor.
The molten slag filtrate the preparation method comprises the following steps: by secondary filter filter residue and 90 DEG C of water in bubbling or strong mixing, pressed Solid waste and molten slag filtrate are obtained after filter.
Embodiment two
A method of sodium pyrophosphate being prepared using crude product sodium pyrophosphate, its step are as follows:
(1) crude product sodium pyrophosphate washing mashing:
1. previous cleaning: crude product sodium pyrophosphate and sodium pyrophosphate mother liquor being added in the stirred tank with filter plate, in 15 DEG C of temperature Degree is lower to stir 2h, so that hydration reaction occurs for the water in anhydrous sodium pyrophosphate and sodium pyrophosphate mother liquor, forms crystalline hydrate, returns Receive the part water in sodium pyrophosphate mother liquor, at the same in crude product sodium chloride and organic matter wash, enter remaining burnt phosphorus In sour mother liquid of sodium, the purpose of concentrate sodium pyrophosphate mother liquor is played, and sodium pyrophosphate mother liquor is previously cooled to 15 DEG C or less again It is washed, finally obtains mixed liquor;
2. filtering: after mixed liquor is reacted in a stirring kettle and washed completely, extracting or extrude 60% out by filter plate Filtrate, the filtrate for retaining 40% in slurry, avoid solid block in kettle, maintain stirring;
3. mashing discharging: be added immediately into stirred tank after filtering heat sodium pyrophosphate apply mother liquor re-start beat Slurry, so that sodium pyrophosphate dissolution of crystals, obtains diluted sodium pyrophosphate slurries after mixing evenly;
(2) sodium pyrophosphate purifies:
Diluted sodium pyrophosphate slurries and molten slag filtrate are mixed, oxidant is added after completely dissolution, progress oxidation reaction, And activated carbon adsorption oily organic matter and Fe is added by after pH value adjustment to 11 using sodium hydroxide solution3+The colloid of formation is heavy It forms sediment, carries out secondary filter, obtain secondary filter filtrate and secondary filter filter residue, by hydrochloric acid or phosphoric acid by secondary filter filtrate PH value adjustment, by secondary filter filtrate crystallisation by cooling, can be obtained after filtering to 10 and apply sodium pyrophosphate mother liquor and sodium pyrophosphate;
(3) cycling and reutilization of sodium pyrophosphate mother liquor:
The sodium pyrophosphate mother liquor of applying being obtained by filtration in step (2) is divided into according to 1:2 volume ratio and to apply sodium pyrophosphate mother Liquid (1) and apply sodium pyrophosphate mother liquor (2), apply sodium pyrophosphate mother liquor (1) alternative steps (1) 1. in sodium pyrophosphate mother liquor, Apply sodium pyrophosphate mother liquor (2) for step (1) 3. in be beaten.
The active carbon accounts for the 0.06t% of crude product sodium pyrophosphate slurries, active carbon and molten slag filtrate mixed liquor.
The molten slag filtrate the preparation method comprises the following steps: by secondary filter filter residue and 90 DEG C of water in bubbling or strong mixing, pressed Solid waste and molten slag filtrate are obtained after filter.
Embodiment three
A method of sodium pyrophosphate being prepared using crude product sodium pyrophosphate, its step are as follows:
(1) crude product sodium pyrophosphate washing mashing:
1. previous cleaning: crude product sodium pyrophosphate and sodium pyrophosphate mother liquor being added in the stirred tank with filter plate, in 28 DEG C of temperature Degree is lower to stir 1.5h, so that hydration reaction occurs for the water in anhydrous sodium pyrophosphate and sodium pyrophosphate mother liquor, forms crystalline hydrate, Recycle the part water in sodium pyrophosphate mother liquor, at the same in crude product sodium chloride and organic matter wash, enter remaining coke In phosphoric acid mother liquid of sodium, the purpose of concentrate sodium pyrophosphate mother liquor is played, and removes in its reaction process reaction heat or by burnt phosphorus Sour mother liquid of sodium is previously cooled to 15 DEG C or less and is washed again, finally obtains mixed liquor;
2. filtering: after mixed liquor is reacted in a stirring kettle and washed completely, extracting or extrude 70% out by filter plate Filtrate, the filtrate for retaining 30% in slurry, avoid solid block in kettle, maintain stirring;
3. mashing discharging: be added immediately into stirred tank after filtering heat sodium pyrophosphate apply mother liquor re-start beat Slurry, so that sodium pyrophosphate dissolution of crystals, obtains diluted sodium pyrophosphate slurries after mixing evenly;
(2) sodium pyrophosphate purifies:
Diluted sodium pyrophosphate slurries and molten slag filtrate are mixed, oxidant is added after completely dissolution, progress oxidation reaction, And activated carbon adsorption oily organic matter and Fe is added by after pH value adjustment to 12 using sodium hydroxide solution3+The colloid of formation is heavy It forms sediment, carries out secondary filter, obtain secondary filter filtrate and secondary filter filter residue, by hydrochloric acid or phosphoric acid by secondary filter filtrate PH value adjustment, by secondary filter filtrate crystallisation by cooling, can be obtained after filtering to after 10 and apply sodium pyrophosphate mother liquor and pyrophosphoric acid Sodium;
(3) cycling and reutilization of sodium pyrophosphate mother liquor:
The sodium pyrophosphate mother liquor of applying being obtained by filtration in step (2) is divided into according to the volume ratio of 1:3.2 and applies pyrophosphoric acid Mother liquid of sodium (1) and apply sodium pyrophosphate mother liquor (2), apply sodium pyrophosphate mother liquor (1) alternative steps (1) 1. in sodium pyrophosphate it is female Liquid, apply sodium pyrophosphate mother liquor (2) for step (1) 3. in be beaten.
The active carbon accounts for the 0.08wt% of crude product sodium pyrophosphate slurries, active carbon and molten slag filtrate mixed liquor.
The molten slag filtrate the preparation method comprises the following steps: by secondary filter filter residue and 85 DEG C of water in bubbling or strong mixing, pressed Solid waste and molten slag filtrate are obtained after filter.
The further filter plate includes sheet frame 14 and filtering plate body 15, sheet frame include cirque structure top plate 16, The bottom plate 17 of cirque structure and the circle side wall 18 being fixed between top plate and bottom plate, the thickness h 1 of side wall are less than top plate Wall wide h2, the wall wide h2 of top plate are equal to the wall wide h3 of bottom plate, the cavity that top plate and bottom plate is arranged in filtering plate body and side wall is surrounded Interior, the filtering plate body includes two filtering board groups, and each filtering board group includes the first filter plate 19 and the second filter plate 20, the The lower surface of one filter plate is uniformly provided with several first raised lines 21, forms the first groove 22 between two adjacent the first raised lines, The upper surface of second filter plate is uniformly provided with several second raised lines 23, forms the second groove between two adjacent the second raised lines 24, the width of the first raised line is L1, and the width of the first groove is L2, and the width of the second raised line is L3, and the width of the second groove is L4, L1=L3 > L2=L4, the first filter plate are placed in the top of the second filter plate, and the first raised line and the second raised line are staggeredly set It sets, is pressed together on the first raised line of the first filter plate on the second groove of the second filter plate, the second raised line pressure of the second filter plate It closes on the first groove of the first filter plate, two filtering board group mirror settings, the second filter plate of two filtering board groups is mutual Contact.
Further, the aperture of first filter plate is greater than the aperture of the second filter plate.
Further, the stir chamber cavity wall of the stirred tank is equipped with the first heat tape 25, on the side wall of the sheet frame Equipped with second heat tape 26 of circle, the bottom plate of sheet frame is equipped at least 1 27 electric heating tubes of circle.The structure setting of filter plate, greatly Width increases the filter effect of filter plate, reduces impurity content in filtrate, and the difficulty of subsequent concentration processing is reduced with this, same with this When, the reasonable distribution heating region in stirred tank makes to be uniformly heated, and reacts more complete.
The structure setting of filter plate is added significantly to the filter effect of filter plate, reduces impurity content in filtrate, is dropped with this The difficulty of low subsequent concentration processing, at the same time, the reasonable distribution heating region in stirred tank makes to be uniformly heated, reaction More completely.

Claims (4)

1. a kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate, it is characterized in that, it the steps include:
(1) crude product sodium pyrophosphate washing mashing:
1. previous cleaning: crude product sodium pyrophosphate and sodium pyrophosphate mother liquor being added in the stirred tank with filter plate, in 0-30 DEG C of temperature Lower stirring 0.5-4h forms crystalline hydrate so that hydration reaction occurs for the water in anhydrous sodium pyrophosphate and sodium pyrophosphate mother liquor, Recycle the part water in sodium pyrophosphate mother liquor, at the same in crude product sodium chloride and organic matter wash, enter remaining coke In phosphoric acid mother liquid of sodium, the purpose of concentrate sodium pyrophosphate mother liquor is played, and removes in its reaction process reaction heat or by burnt phosphorus Sour mother liquid of sodium is previously cooled to 15 DEG C or less and is washed again, finally obtains mixed liquor;
2. filtering: after mixed liquor is reacted in a stirring kettle and washed completely, extracting or extrude the filter of 50%-80% out by filter plate Liquid, the filtrate for retaining 20-50% in slurry, avoid solid block in kettle, maintain stirring;
3. mashing discharging: the sodium pyrophosphate that heat is added after filtering into stirred tank immediately applies mother liquor and re-starts mashing, So that sodium pyrophosphate dissolution of crystals, obtains diluted sodium pyrophosphate slurries after mixing evenly;
(2) sodium pyrophosphate purifies:
Diluted sodium pyrophosphate slurries and molten slag filtrate are mixed, oxidant is added after completely dissolution, carry out oxidation reaction and made After pH value is adjusted to 11-12 with sodium hydroxide solution, activated carbon adsorption oily organic matter and Fe is added3+The colloid of formation is heavy It forms sediment, carries out secondary filter, obtain secondary filter filtrate and secondary filter filter residue, by hydrochloric acid or phosphoric acid by secondary filter filtrate After pH value is adjusted to 9.8-10.5, by secondary filter filtrate crystallisation by cooling, can be obtained after filtering apply sodium pyrophosphate mother liquor and Sodium pyrophosphate;
(3) cycling and reutilization of sodium pyrophosphate mother liquor:
Apply sodium pyrophosphate mother liquor according to 1:(1-4 for what is be obtained by filtration in step (2)) volume ratio be divided into first and apply burnt phosphorus Sour mother liquid of sodium and second applies sodium pyrophosphate mother liquor, first apply sodium pyrophosphate mother liquor alternative steps (1) 1. in sodium pyrophosphate Mother liquor, second apply sodium pyrophosphate mother liquor for step (1) 3. in be beaten;
The molten slag filtrate the preparation method comprises the following steps: by secondary filter filter residue and 80-100 DEG C of drum bubble or strong mixing, carry out filters pressing After obtain solid waste and molten slag filtrate.
2. a kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate as described in claim 1, it is characterized in that, the work Property charcoal accounts for the 0.02-0.1wt% of crude product sodium pyrophosphate slurries, active carbon and molten slag filtrate mixed liquor.
3. a kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate as described in claim 1, it is characterized in that, the oxygen Agent is hydrogen peroxide, sodium chlorate, chlorine dioxide, combination one or more in ozone.
4. a kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate as described in claim 1, it is characterized in that, step (1) wash mill is used in, the wash mill includes stirred tank, waste tank and dissolution kettle, is equipped with and stirs in the stirred tank It mixes leaf, filter plate is equipped with below paddle, filter plate will be separated into stir chamber and filter chamber in stirred tank, stirred tank is equipped with the One feed inlet, second charging aperture, suction filtration mouth and discharge port, first charging aperture and second charging aperture are located at the top of stirred tank, with Stir chamber is connected, and suction filtration mouth is located at the bottom of stirred tank, is connected with chamber is filtered, and discharge port is located at first charging aperture and filters Between mouthful, it is connected with stir chamber;Suction filtration mouth is connected by first pipe with the third feed inlet of waste tank, and discharge port is logical Second pipe is crossed to be connected with dissolution kettle.
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CN106335889A (en) * 2016-08-18 2017-01-18 宜宾天原集团股份有限公司 Method for producing sodium tripolyphosphate by utilization of crude sodium pyrophosphate

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CN101121506A (en) * 2007-07-30 2008-02-13 四川宏达股份有限公司 Technique for preparing sodium pyrophosphate from wet method phosphoric acid
CN101712466A (en) * 2008-10-06 2010-05-26 天津市化学试剂研究所 Method for preparing edible crystalline sodium pyrophosphate
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CN106335889A (en) * 2016-08-18 2017-01-18 宜宾天原集团股份有限公司 Method for producing sodium tripolyphosphate by utilization of crude sodium pyrophosphate

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