CN106348269A - Comprehensive utilization method of phosphoric acid waste liquid and sodium hydroxide waste liquid - Google Patents
Comprehensive utilization method of phosphoric acid waste liquid and sodium hydroxide waste liquid Download PDFInfo
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- CN106348269A CN106348269A CN201610776823.2A CN201610776823A CN106348269A CN 106348269 A CN106348269 A CN 106348269A CN 201610776823 A CN201610776823 A CN 201610776823A CN 106348269 A CN106348269 A CN 106348269A
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- Prior art keywords
- sodium hydroxide
- discharge liquid
- waste liquid
- phosphate
- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
- C01B25/303—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates with elimination of impurities
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention relates to a comprehensive utilization method of a phosphoric acid waste liquid and a sodium hydroxide waste liquid. The method specifically comprises the following steps: heating the phosphoric acid waste liquid to 40-60 DEG C, adding the sodium hydroxide waste liquid dropwise into the phosphoric acid waste liquid at the stirring speed of 50-80rpm until the pH value of a reaction liquid is 3.5-4.7, obtaining a slurry containing sodium dihydrogen phosphate, adding an activated carbon and sodium carboxymethylcellulose into the slurry, stirring for 1-2 hours, filtering, collecting a filtrate, cooling the filtrate to 20-30 DEG C, adding ethyl alcohol, standing and crystalizing to obtain a crystallization mother liquor, filtering the crystallization mother liquor, and drying a filter cake to obtain the sodium dihydrogen phosphate. According to the preparation method, the process flow is short, the operation is convenient, the product purity is high, the yield is high, the production cost is low, the industrial production is easy to implement, and meanwhile, the phosphoric acid waste liquid and the sodium hydroxide waste liquid are turned into treasure.
Description
Technical field
The present invention relates to the method for comprehensive utilization of a kind of phosphate discharge liquid and sodium hydroxide waste liquor, specially one kind utilize phosphoric acid
The method that waste liquid and sodium hydroxide waste liquor prepare sodium dihydrogen phosphate, belongs to chemical technology field.
Background technology
Sodium dihydrogen phosphate, colourless iris crystallization, it is a kind of important phosphate product, tool has been widely used, can use
In boiler water process, plating, process hides, baking powder, color additive, detergent, acidity buffer agent etc., be also produce sodium hexameta phosphate and
The raw material of condensed phosphate.Sodium dihydrogen phosphate also is used as the fire retardant of fabric, timber and paper, anti-creasing agent etc.；In food work
Fermentation raw material, acidic flavoring agent, the stabilizer of meat productss and binding agent etc. are used on industry.
Chinese invention patent " a kind of method that phosphoric acid by wet process prepares sodium dihydrogen phosphate ", publication number cn103787293a,
Disclose a kind of reaction under 40～90 DEG C of stirring conditions using phosphoamide and phosphoric acid by wet process and obtain intermediate, then by this intermediate
React 20～100min with sodium hydroxide under 40～90 DEG C of stirring conditions, sodium dihydrogen phosphate serosity is cooled to temperature≤40 DEG C,
Crystallisation by cooling, after filtration cakes torrefaction after centrifugal filtration, obtains sodium dihydrogen phosphate product.Phosphoric acid by wet process used is using centrifugation or filter pressing
Method remove solid impurity.
But, there is obvious defect and deficiency in the method that above-mentioned phosphoric acid by wet process prepares sodium dihydrogen phosphate: (1) using from
The method of the heart or filter pressing only removes solid impurity it is impossible to remove soluble metal ion in phosphoric acid by wet process, such as magnesium ion, calcium from
Son, in phosphoric acid by wet process, these soluble metal ions can disturb the preparation of sodium dihydrogen phosphate, and reduces the purity of sodium dihydrogen phosphate；
(2) sodium dihydrogen phosphate serosity is cooled to temperature≤40 DEG C crystallization, and when 40 DEG C, the dissolubility of sodium dihydrogen phosphate is up to 133g, knot
The substantial amounts of sodium dihydrogen phosphate not crystallizing precipitation can be remained in brilliant mother solution, cause the loss of sodium dihydrogen phosphate, reduce finished product
Yield, leads to production cost high.
Content of the invention
In order to solve problems of the prior art, the present invention provides a kind of new side preparing sodium dihydrogen phosphate
Method, the present invention, with phosphate discharge liquid and sodium hydroxide waste liquor as raw material, reduces production cost it is achieved that turning waste into wealth；Originally simultaneously
The preparation method technological process of invention is short, easy and simple to handle, and finished product purity is high, high income is it is easy to industrialized production.
The technical scheme realizing purpose of the present invention employing is:
A kind of phosphate discharge liquid and the method for comprehensive utilization of sodium hydroxide waste liquor, comprise the steps:
1) phosphate discharge liquid is heated to 40～60 DEG C, under 50～80rpm mixing speed, the Deca hydrogen-oxygen in phosphate discharge liquid
Change waste liquor of sodium, be 3.5～4.7 to reactant liquor ph value, obtain the serosity of phosphoric acid sodium dihydrogen；
2) to step 1) add activated carbon and sodium carboxymethyl cellulose in the serosity prepared, stir 1～2h, filter, collect
Filtrate；
3) by step 2) filtrate be cooled to 20～30 DEG C, add ethanol, stand still for crystals, obtain crystalline mother solution；
4) by step 3) crystalline mother solution filter, obtain sodium dihydrogen phosphate after filtration cakes torrefaction.
Preferably, step 1) mass concentration of phosphoric acid is 15～30% in described phosphate discharge liquid, described sodium hydroxide waste liquor
The mass concentration 10～28% of middle sodium hydroxide.
Preferably, step 2) described activated carbon quality be phosphate discharge liquid quality 3～6%.
Preferably, step 2) described sodium carboxymethyl cellulose quality be phosphate discharge liquid quality 1～2%.
Preferably, step 3) described ethanol quality be phosphate discharge liquid quality 15～30%.
Preferably, step 3) described in stand still for crystals the time be 2～5h.
Preferably, step 4) described drying temperature be 100～105 DEG C.
The primary raw material that the present invention prepares sodium dihydrogen phosphate is 15～30wt% phosphate discharge liquid and 10～28wt% hydroxide
Waste liquor of sodium, it is achieved that phosphate discharge liquid and sodium hydroxide waste liquor refuse reclamation, greatly reduces the production cost of sodium dihydrogen phosphate,
Avoid the discharge of phosphate discharge liquid and sodium hydroxide waste liquor simultaneously.
The present invention using to by the way of Deca sodium hydroxide waste liquor in phosphate discharge liquid, when reactant liquor ph value is 3.5～4.7
When, stop Deca sodium hydroxide waste liquor, control prepared product to be sodium dihydrogen phosphate.When addition 3～6% phosphoric acid in serosity
Pigment in the adsorbable serosity of activated carbon of waste liquid quality；When the sodium carboxymethyl cellulose adding 1～2% phosphate discharge liquid quality,
Carboxymethyl cellulose by chelating with soluble metal ion, can soluble metal ion in active adsorption sediment slurry,
Remove pigment and the soluble metal ion in serosity by activated carbon and sodium carboxymethyl cellulose respectively, improve sodium dihydrogen phosphate
Purity.
Sodium dihydrogen phosphate is soluble in water, but does not dissolve in ethanol, and the present invention passes through to add ethanol in crystalline mother solution, ethanol
Adding the polarity reducing crystalline mother solution, thus reducing dissolubility in crystalline mother solution for the sodium dihydrogen phosphate, promoting biphosphate
Sodium crystallization separates out, and improves the yield of sodium dihydrogen phosphate.The mass concentration of the ethanol adding in crystalline mother solution of the present invention is 95%.
Compared with prior art, the beneficial effects of the present invention is:
1st, the present invention adds activated carbon and sodium carboxymethyl cellulose in the serosity of phosphoric acid sodium dihydrogen, and activated carbon has
Inhale decolorization；Sodium carboxymethyl cellulose has flocculation, chelation, can effectively adsorb soluble metal ion and incite somebody to action
Its precipitation, can effectively remove the soluble metal ion in the serosity of sodium dihydrogen phosphate, activated carbon and sodium carboxymethyl cellulose are altogether
With the purity improving sodium dihydrogen phosphate.
2nd, the crystallization temperature of the present invention is 20～30 DEG C, close to room temperature, is easy to crystallization operation and reduces sodium dihydrogen phosphate and exist
Dissolubility in crystalline mother solution；Additionally, adding the ethanol of 15～30% phosphate discharge liquid quality in crystalline mother solution, reduce crystallization
The polarity of mother solution, reduces dissolubility in crystalline mother solution for the sodium dihydrogen phosphate further so as to overwhelming majority crystallization separates out, reduces
The loss of sodium dihydrogen phosphate, improves the yield of finished product sodium dihydrogen phosphate, reduces production cost.
3rd, the primary raw material preparing sodium dihydrogen phosphate is phosphate discharge liquid and sodium hydroxide waste liquor it is achieved that phosphate discharge liquid and hydrogen
Oxidation waste liquor of sodium is turned waste into wealth, and not only greatly reduces the production cost of sodium dihydrogen phosphate, avoids phosphate discharge liquid and hydrogen simultaneously
The discharge of oxidation waste liquor of sodium, is effectively protected environment.
4th, preparation method technological process of the present invention is short, easy and simple to handle, mild condition, safe it is easy to industrialized production.
Specific embodiment
For making those skilled in the art can be better understood from the present invention and can be practiced, with reference to being embodied as
The present invention is further elaborated for example.
Embodiment 1
1) the phosphate discharge liquid 1000g that mass concentration is 20% is heated to 50 DEG C, under 60rpm mixing speed, to phosphoric acid
In waste liquid, Deca mass concentration is 20% sodium hydroxide waste liquor, is 4.5 to reactant liquor ph value, obtains the slurry of phosphoric acid sodium dihydrogen
Liquid；
2) to step 1) add activated carbon 40g and sodium carboxymethyl cellulose 10g in the serosity prepared, stir 2h, filter, receive
Collection filtrate；
3) by step 2) filtrate be cooled to 20 DEG C, add 95wt% ethanol 250g, stand still for crystals 4h, obtain crystallization female
Liquid；
4) by step 3) crystalline mother solution filter, 102 DEG C of dryings of filter cake, obtain white sodium dihydrogen phosphate 232g.
Embodiment 2
1) the phosphate discharge liquid 1000g that mass concentration is 15% is heated to 60 DEG C, under 80rpm mixing speed, to phosphoric acid
In waste liquid, Deca mass concentration is 10% sodium hydroxide waste liquor, is 4.1 to reactant liquor ph value, obtains the slurry of phosphoric acid sodium dihydrogen
Liquid；
2) to step 1) add activated carbon 40g and sodium carboxymethyl cellulose 20g in the serosity prepared, stir 1.2h, filter,
Collect filtrate；
3) by step 2) filtrate be cooled to 25 DEG C, add 95wt% ethanol 300g, stand still for crystals 5h, obtain crystallization female
Liquid；
4) by step 3) crystalline mother solution filter, 105 DEG C of dryings of filter cake, obtain white sodium dihydrogen phosphate 165g.
Embodiment 3
1) the phosphate discharge liquid 1000g that mass concentration is 25% is heated to 50 DEG C, under 50rpm mixing speed, to phosphoric acid
In waste liquid, Deca mass concentration is 25% sodium hydroxide waste liquor, is 3.5 to reactant liquor ph value, obtains the slurry of phosphoric acid sodium dihydrogen
Liquid；
2) to step 1) add activated carbon 30g and sodium carboxymethyl cellulose 18g in the serosity prepared, stir 1.8h, filter,
Collect filtrate；
3) by step 2) filtrate be cooled to 30 DEG C, add 95wt% ethanol 200g, stand still for crystals 3h, obtain crystallization female
Liquid；
4) by step 3) crystalline mother solution filter, 101 DEG C of dryings of filter cake, obtain white sodium dihydrogen phosphate 260g.
Embodiment 4
1) the phosphate discharge liquid 1000g that mass concentration is 20% is heated to 40 DEG C, under 60rpm mixing speed, to phosphoric acid
In waste liquid, Deca mass concentration is 28% sodium hydroxide waste liquor, is 4.3 to reactant liquor ph value, obtains the slurry of phosphoric acid sodium dihydrogen
Liquid；
2) to step 1) add activated carbon 50g and sodium carboxymethyl cellulose 15g in the serosity prepared, stir 1h, filter, receive
Collection filtrate；
3) by step 2) filtrate be cooled to 20 DEG C, add 95wt% ethanol 200g, stand still for crystals 2h, obtain crystallization female
Liquid；
4) by step 3) crystalline mother solution filter, 100 DEG C of dryings of filter cake, obtain white sodium dihydrogen phosphate 226g.
Embodiment 5
1) the phosphate discharge liquid 1000g that mass concentration is 30% is heated to 60 DEG C, under 70rpm mixing speed, to phosphoric acid
In waste liquid, Deca mass concentration is 20% sodium hydroxide waste liquor, is 4.7 to reactant liquor ph value, obtains the slurry of phosphoric acid sodium dihydrogen
Liquid；
2) to step 1) add activated carbon 60g and sodium carboxymethyl cellulose 12g in the serosity prepared, stir 1.5h, filter,
Collect filtrate；
3) by step 2) filtrate be cooled to 25 DEG C, add 95wt% ethanol 150g, stand still for crystals 3h, obtain crystallization female
Liquid；
4) by step 3) crystalline mother solution filter, 102 DEG C of dryings of filter cake, obtain white sodium dihydrogen phosphate 323g.
Claims (7)
1. the method for comprehensive utilization of a kind of phosphate discharge liquid and sodium hydroxide waste liquor is it is characterised in that comprise the steps:
1) phosphate discharge liquid is heated to 40～60 DEG C, under 50～80rpm mixing speed, the Deca sodium hydroxide in phosphate discharge liquid
Waste liquid, is 3.5～4.7 to reactant liquor ph value, obtains the serosity of phosphoric acid sodium dihydrogen；
2) to step 1) add activated carbon and sodium carboxymethyl cellulose in the serosity prepared, stir 1～2h, filter, collect filtrate；
3) by step 2) filtrate be cooled to 20～30 DEG C, add ethanol, stand still for crystals, obtain crystalline mother solution；
4) by step 3) crystalline mother solution filter, obtain sodium dihydrogen phosphate after filtration cakes torrefaction.
2. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
1) in described phosphate discharge liquid, the mass concentration of phosphoric acid is 15～30%, the mass concentration of sodium hydroxide in described sodium hydroxide waste liquor
10～28%.
3. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
2) quality of described activated carbon is the 3～6% of phosphate discharge liquid quality.
4. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
2) quality of described sodium carboxymethyl cellulose is the 1～2% of phosphate discharge liquid quality.
5. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
3) quality of described ethanol is the 15～30% of phosphate discharge liquid quality.
6. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
3) time that stands still for crystals described in is 2～5h.
7. the method for comprehensive utilization of phosphate discharge liquid according to claim 1 and sodium hydroxide waste liquor is it is characterised in that step
4) temperature of described drying is 100～105 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610776823.2A CN106348269A (en) | 2016-08-30 | 2016-08-30 | Comprehensive utilization method of phosphoric acid waste liquid and sodium hydroxide waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610776823.2A CN106348269A (en) | 2016-08-30 | 2016-08-30 | Comprehensive utilization method of phosphoric acid waste liquid and sodium hydroxide waste liquid |
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| CN201610776823.2A Pending CN106348269A (en) | 2016-08-30 | 2016-08-30 | Comprehensive utilization method of phosphoric acid waste liquid and sodium hydroxide waste liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453710A (en) * | 2020-05-20 | 2020-07-28 | 无锡中天固废处置有限公司 | Method for preparing disodium hydrogen phosphate from metal-containing phosphoric acid waste liquid of switch production process |
| CN112678788A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891172A (en) * | 2010-07-17 | 2010-11-24 | 天津市化学试剂研究所 | Preparation method for food grade disodium hydrogen phosphate |
-
2016
- 2016-08-30 CN CN201610776823.2A patent/CN106348269A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891172A (en) * | 2010-07-17 | 2010-11-24 | 天津市化学试剂研究所 | Preparation method for food grade disodium hydrogen phosphate |
Non-Patent Citations (2)
| Title |
|---|
| 范青生等: "《保健食品配方原理与依据》", 31 January 2007, 中国医药科技出版社 * |
| 许晓文等: "《定量化学分析》", 30 April 2016, 南开大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678788A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
| CN112678788B (en) * | 2019-10-18 | 2022-10-11 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
| CN111453710A (en) * | 2020-05-20 | 2020-07-28 | 无锡中天固废处置有限公司 | Method for preparing disodium hydrogen phosphate from metal-containing phosphoric acid waste liquid of switch production process |
| CN111453710B (en) * | 2020-05-20 | 2023-05-12 | 无锡中天固废处置有限公司 | Method for preparing disodium hydrogen phosphate from metal-containing phosphoric acid waste liquid in switch production process |
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Application publication date: 20170125 |