CN107162935A - The recovery method of phosphorus-containing compound in useless chemical polishing agent - Google Patents
The recovery method of phosphorus-containing compound in useless chemical polishing agent Download PDFInfo
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- CN107162935A CN107162935A CN201710392425.5A CN201710392425A CN107162935A CN 107162935 A CN107162935 A CN 107162935A CN 201710392425 A CN201710392425 A CN 201710392425A CN 107162935 A CN107162935 A CN 107162935A
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- Prior art keywords
- chemical polishing
- polishing agent
- recovery method
- mother liquor
- urea
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
- C07C273/14—Separation; Purification; Stabilisation; Use of additives
- C07C273/16—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B15/00—Organic phosphatic fertilisers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The present invention provides a kind of recovery method of phosphorus-containing compound in useless chemical polishing agent, comprises the following steps：Acetic acid and nitric acid in the useless chemical polishing agent of extraction；By the useless chemical polishing agent concentration after extraction；Crystallized after urea, reaction completely will be added in useless chemical polishing agent after concentration, isolated PHOSPHORIC ACID TECH.GRADE urea and crystalline mother solution；Precipitating reagent will be added in crystalline mother solution, sediment separate out is purified mother liquor；By the purification mother liquor concentrations, Crystallization Separation obtains feed grade urea phosphate and secondary crystallization mother liquor.Method recovery product purity provided by the present invention is high, and quality is good, can not only reach that industrial circle uses rank, moreover it is possible to use as the additive of feed or the raw material of high concentration N-P composite fertilizer.The production process of this method is simple, it is easy to operate, and easy control of reaction conditions, cost is low, and the rate of recovery to phosphorus is high, large-scale production is easily realized, with obviously economic benefit and environmental benefit.
Description
Technical field
The present invention relates to a kind of recovery method of phosphorus-containing compound in useless chemical polishing agent.
Background technology
The etch in the polishing solution that the corrosive agent, oxidant, additive of reasonable mixture ratio are constituted of metal material or product, warp
After generation series reaction, surface becomes clean light, referred to as chemical polishing.Most of chemical polishing of aluminium and aluminium alloy is used
Phosphoric acid based sols are carried out, the solution based on the phosphoric acid of 70% (mass percent).Conventional be phosphoric acid, sulfuric acid, nitric acid or
Acetic acid mixed liquor, the high solution of phosphorus acid content can make the surface after mechanical polishing reach the height light suitable with electropolishing
Degree, for fine aluminium, zinc content is not higher than Al-Mg-Zn and the Al-Cu-Mg alloy that 8%, copper content is not higher than 4%.
Substantial amounts of waste liquid is produced in polishing process, mainly containing phosphoric acid, acetic acid, heavy metal ion of higher concentration etc. has
Harmful chemical substance, with very strong corrosivity, belongs to《National Hazard waste register》HW34 classes.Before this, this is typically handled
The method for planting chemical polishing agent is to add lime to neutralize, waste landfills.The method can produce a large amount of phosphorus containing sludges, and increase is filled into
This, or even environmental pollution can be caused.
At present, for some existing Patents of comprehensive utilization and document report of such waste phosphoric acid, such as patent CN
101456547 B, as nertralizer, by step-by-step precipitation method, realize purification and the fertilizer grade phosphorus of heavy metal ion using milk of lime
The preparation of the product of sour hydrogen calcium, generates contain substantial amounts of aluminium salt in the calcium monohydrogen phosphate come in this way, and phosphoric acid hydrogen
The market outlet of calcium is not good, and added value of product is relatively low.Patent 201610795470.0 proposes a kind of aluminium polishing waste phosphoric acid liquid resource
Change recovery method, precipitation removes aluminium in the form of fluorine-containing solution and sodium salt is added with ice crystal, then is given birth to calcium salt three-step precipitation method
Calcium monohydrogen phosphate and general calcium are produced, phosphoric acid is fully used, but precipitation separation is complicated, added value of product is low.
The content of the invention
, being capable of the useless chemical polishing of high-efficiency environment friendly processing it is an object of the invention to provide one kind for defect of the prior art
The recovery method of agent.
The present invention provides a kind of recovery method of phosphorus-containing compound in useless chemical polishing agent, comprises the following steps：
Acetic acid and nitric acid in the useless chemical polishing agent of extraction；
By the useless chemical polishing agent concentration after extraction；
Crystallized after urea, reaction completely will be added in useless chemical polishing agent after concentration, isolated PHOSPHORIC ACID TECH.GRADE urea
And crystalline mother solution；
Precipitating reagent will be added in crystalline mother solution, sediment separate out is purified mother liquor；
By the purification mother liquor concentrations, Crystallization Separation obtains feed grade urea phosphate and secondary crystallization mother liquor.
Method provided by the present invention mainly reclaims phosphorus-containing compound in useless chemical polishing agent in the form of urea phosphate, its
Purity is high, and quality is good, can not only reach that industrial circle uses rank, moreover it is possible to answered as the additive or high concentration N-P of feed
The raw material in Hefei is used.Extensively, added value is high for its product purpose.
This method finally only produces a small amount of sludge simultaneously, reduces landfill expense.And production process is simple, it is easy to
Operation, easy control of reaction conditions, cost is low, and the rate of recovery to phosphorus is high, large-scale production is easily realized, with obviously
Economic benefit and environmental benefit.
Embodiment
The solution of the present invention is explained in detail below, it will be understood to those of skill in the art that example is only used for below
The present invention is explained, and is not considered as limiting the invention.
One aspect of the present invention provides a kind of recovery method of phosphorus-containing compound in useless chemical polishing agent, comprises the following steps：
Acetic acid and nitric acid in the useless chemical polishing agent of extraction；
By the useless chemical polishing agent concentration after extraction；
Urea will be added in useless chemical polishing agent after concentration, crystallized after reaction, isolated PHOSPHORIC ACID TECH.GRADE urea and knot
Brilliant mother liquor；
Precipitating reagent will be added in crystalline mother solution, sediment separate out is purified mother liquor；
By the purification mother liquor concentrations, Crystallization Separation obtains feed grade urea phosphate and secondary crystallization mother liquor.
According to a particular embodiment of the invention, in the useless chemical polishing agent of the extract and separate in acetic acid and nitric acid, using extraction
Agent is taken to be extracted, the extractant includes at least one of tributyl phosphate, trioctyl phosphate, and diluent is including kerosene etc..
According to a particular embodiment of the invention, the mode of the extraction is using more than two-stage extraction or two-stage extraction.
According to a particular embodiment of the invention, the addition of the urea is phosphorus in the useless chemical polishing agent after the concentration
0.9~1.1 times of the amount of acid substance, the weight/mass percentage composition of the urea is more than 98%.
According to a particular embodiment of the invention, after the concentration useless chemical polishing agent and the temperature of urea reaction be 30~
80 DEG C, 30~120min of mixing time, reacted crystallization is by the way of crystallisation by cooling, and the temperature of the crystallisation by cooling is less than
Equal to 30 DEG C.
According to a particular embodiment of the invention, the useless chemical polishing agent after the concentration enters one with being crystallized after urea reaction
Step includes centrifugal filtration, washs, and dries, obtains PHOSPHORIC ACID TECH.GRADE urea and crystalline mother solution.The centrifugal filtration, washing is dried
Method can use method well known to those skilled in the art.
According to a particular embodiment of the invention, the precipitating reagent is sulfide, and the weight/mass percentage composition of the sulfide is
More than 98%.The amount for adding precipitating reagent is that precipitation is no longer produced into crystalline mother solution i.e. only.The present invention adds precipitating reagent can
Remove the partly or completely foreign ion such as Cu, Pb, As.
According to a particular embodiment of the invention, the sulfide include hydrogen sulfide, ammonium sulfide or vulcanized sodium at least it
One.
According to a particular embodiment of the invention, by the mode of the purification mother liquor concentrations using vacuum concentration, the vacuum
Thickening temperature is 60~80 DEG C, and vacuum is more than or equal to 0.06Mpa.
According to a particular embodiment of the invention, by crystallization after the purification mother liquor concentrations by the way of crystallisation by cooling, institute
Stating crystallisation by cooling also needs to add urea phosphate crystal seed, and addition is 0.5~5g/L.
According to a particular embodiment of the invention, will be crystallized after the purification mother liquor concentrations also includes after crystallization, is separated by filtration,
Dry, obtain feed grade urea phosphate and secondary crystallization mother liquor.Described to be separated by filtration, dry method can use people in the art
Method known to member.
According to a particular embodiment of the invention, by the useless chemical polishing agent after the extraction be concentrated into density for 1.4~
1.6g/mL, and by it is described purification mother liquor concentrations to phosphorus content be 14~15.5%.
Useless chemical polishing agent of the present invention can be regarded as phosphoric acid-acetic acid system chemical polishing agent commonly used in this field and give up
Liquid.It is preferred that, in the useless chemical polishing agent total phosphorus content be 122~200g/L, acetic acid 0.7~5%, nitric acid 0.1~
0.3%.The content of useless chemical polishing agent other compositions of the present invention is is not limited in the present invention.
Embodiment 1
The useless chemical polishing agent 1000mL of phosphoric acid-acetic acid system is taken, its relative density is 1.21, and wherein total phosphorus content is 122g/
L, acetic acid 0.7%, nitric acid 0.1%, aluminium content 0.9g/L, Fe content 6mg/L, Cu content 5mg/L, Zn content 4mg/L, Pb contains
Measure 0.05mg/L.
(1) first using 15% tributyl phosphate and 85% kerosene as extractant, compared to O/A=1/2, under normal temperature
Two-stage extract and separate removes the acetic acid and nitric acid in useless chemical polishing agent, and the loss late of phosphorus is 6%；
(2) it is 1.50g/mL and then raffinate to be concentrated by evaporation to density；
(3) reactor is poured into after cooling down, then is slowly added to 253g agricultural grades (98%) urea (urea and phosphorus while stirring
The mol ratio of acid is 1.1：1), at 80 DEG C, 30min, reaction synthesis urea phosphate are stirred；
(4) 25 DEG C of crystallization 2h are cooled to after question response is complete, centrifugal filtration, 50 DEG C of drying obtain 447.3g urea phosphates, produced
Product meet technical grade primary standard；
(5) mother liquor is added the ammonium sulfide of 98% metering by total metalses, and precipitation reaction is filtrated to get purification mother liquor；
(6) previous step end gained filtrate is sent into cold boiler, 60 DEG C of keeping temperature, vacuum 0.09Mpa, concentration
It is 14.0% to being concentrated into phosphorous, cools down and add 0.5g/L urea phosphate crystal seeds and stir and be cooled to 30 DEG C of crystallization 1h, filtering point
From 50 DEG C of drying produce 96.7g urea phosphates, product meets feed grade standard.
Two-step crystallization, there are urea phosphate product 544.0g, and the direct yield of phosphoric acid reaches 86.7%, and remaining a small amount of mother liquor makees fertilizer
Material is used.
Embodiment 2
The useless chemical polishing agent 500mL of phosphoric acid-acetic acid system is taken, its relative density is 1.35, and wherein total phosphorus content is 200.5g/
L, acetic acid 5%, nitric acid 0.3%, aluminium content 3.9g/L, Fe content 10mg/L, Cu content 7mg/L, Zn content 15mg/L, Pb content
0.1mg/L。
(1) first using 50% trioctyl phosphate and 50% tri-n-octyl amine (TOA) as extractant, compared to O/A=1/
4, three-level extract and separate removes the acetic acid and nitric acid in useless chemical polishing agent under normal temperature, and the loss late of phosphorus is 6%；
(2) it is 1.60g/mL and then raffinate to be concentrated by evaporation to density；
(3) cool down after pour into reactor, then be slowly added to while stirring 167.1g agricultural grades (98%) urea (urea with
The mol ratio of phosphoric acid is 0.9:1), at 30 DEG C, 120min, reaction synthesis urea phosphate are stirred；
(4) 25 DEG C of crystallization 2h are cooled to after question response is complete, centrifugal filtration, 50 DEG C of drying obtain 368.6g urea phosphates, produced
Product meet technical grade primary standard；
(5) mother liquor is added the ammonium sulfide of 100% metering by total metalses, and precipitation reaction is filtrated to get purification mother liquor；
(6) previous step end gained filtrate is sent into cold boiler, 80 DEG C of keeping temperature, vacuum 0.06Mpa, concentration
It is 15.5% to being concentrated into phosphorous, adds 5g/L urea phosphate crystal seeds and stir and be cooled to 30 DEG C of crystallization 1h, be separated by filtration, 50 DEG C of bakings
It is dry, 50.7g urea phosphates are produced, product meets feed grade standard.
Two-step crystallization, there are urea phosphate product 419.3g, and the direct yield of phosphoric acid reaches 84.1%, and remaining a small amount of mother liquor makees fertilizer
Material is used.
The above-described embodiments are merely illustrative of preferred embodiments of the present invention, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, this area ordinary skill technical staff is to the technology of the present invention
In various modifications and improvement that scheme is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (10)
1. the recovery method of phosphorus-containing compound, comprises the following steps in a kind of useless chemical polishing agent：
Acetic acid and nitric acid in the useless chemical polishing agent of extraction；
By the useless chemical polishing agent concentration after extraction；
Crystallized after urea, reaction completely will be added in useless chemical polishing agent after concentration, isolated PHOSPHORIC ACID TECH.GRADE urea and knot
Brilliant mother liquor；
Precipitating reagent will be added in crystalline mother solution, sediment separate out is purified mother liquor；
By the purification mother liquor concentrations, Crystallization Separation obtains feed grade urea phosphate and secondary crystallization mother liquor.
2. recovery method according to claim 1, it is characterised in that acetic acid and nitric acid in the useless chemical polishing agent of extract and separate
In, extracted using extractant, the extractant includes at least one of tributyl phosphate, trioctyl phosphate.
3. recovery method according to claim 1, it is characterised in that the addition of the urea is useless after the concentration
0.9~1.1 times of the amount of phosphoric acid substance in chemical polishing agent.
4. recovery method according to claim 1, it is characterised in that the useless chemical polishing agent and urea after the concentration are anti-
The temperature answered is 30~80 DEG C, 30~120min of mixing time.
5. recovery method according to claim 1, it is characterised in that the useless chemical polishing agent and urea after the concentration are anti-
It should crystallize afterwards by the way of crystallisation by cooling, the temperature of the crystallisation by cooling is less than or equal to 30 DEG C.
6. recovery method according to claim 1, it is characterised in that the precipitating reagent is sulfide.
7. recovery method according to claim 6, it is characterised in that the sulfide include hydrogen sulfide, ammonium sulfide or
At least one of vulcanized sodium.
8. recovery method according to claim 1, it is characterised in that the mode of the purification mother liquor concentrations is used into vacuum
Concentration, the temperature concentrated in vacuo is 60~80 DEG C, and vacuum is more than or equal to 0.06Mpa.
9. recovery method according to claim 1, it is characterised in that by crystallization after the purification mother liquor concentrations using cooling
The mode of crystallization, the crystallisation by cooling also needs to add urea phosphate crystal seed, and addition is 0.5~5g/L.
10. recovery method according to claim 1, it is characterised in that concentrate the useless chemical polishing agent after the extraction
To density be 1.4~1.6g/mL, and by it is described purification mother liquor concentrations to phosphorus content be 14~15.5%.
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| CN201710392425.5A CN107162935B (en) | 2017-05-27 | 2017-05-27 | The recovery method of phosphorus-containing compound in useless chemical polishing agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574069A (en) * | 2020-12-04 | 2021-03-30 | 上海天汉环境资源有限公司 | Resource utilization method of waste phosphoric acid in microelectronic industry |
| CN112827466A (en) * | 2020-12-31 | 2021-05-25 | 深圳市环保科技集团有限公司 | Preparation method and application of aluminum type adsorbent |
| CN115304514A (en) * | 2022-08-17 | 2022-11-08 | 新中天环保股份有限公司 | Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry |
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|---|---|---|---|---|
| CN101456547A (en) * | 2008-12-19 | 2009-06-17 | 深圳市危险废物处理站有限公司 | Comprehensive utilization method of chemical polishing waste phosphoric acid |
| CN105088246A (en) * | 2015-08-13 | 2015-11-25 | 合肥鑫艺达抛光机械有限公司 | Environment-friendly stainless steel chemical polishing agent |
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN106430267A (en) * | 2016-08-31 | 2017-02-22 | 池州西恩新材料科技有限公司 | Resource recycling method for aluminum polishing phosphoric acid waste liquid |
-
2017
- 2017-05-27 CN CN201710392425.5A patent/CN107162935B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456547A (en) * | 2008-12-19 | 2009-06-17 | 深圳市危险废物处理站有限公司 | Comprehensive utilization method of chemical polishing waste phosphoric acid |
| CN105088246A (en) * | 2015-08-13 | 2015-11-25 | 合肥鑫艺达抛光机械有限公司 | Environment-friendly stainless steel chemical polishing agent |
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN106430267A (en) * | 2016-08-31 | 2017-02-22 | 池州西恩新材料科技有限公司 | Resource recycling method for aluminum polishing phosphoric acid waste liquid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574069A (en) * | 2020-12-04 | 2021-03-30 | 上海天汉环境资源有限公司 | Resource utilization method of waste phosphoric acid in microelectronic industry |
| CN112574069B (en) * | 2020-12-04 | 2021-12-28 | 上海天汉环境资源有限公司 | Resource utilization method of waste phosphoric acid in microelectronic industry |
| CN112827466A (en) * | 2020-12-31 | 2021-05-25 | 深圳市环保科技集团有限公司 | Preparation method and application of aluminum type adsorbent |
| CN112827466B (en) * | 2020-12-31 | 2023-01-17 | 深圳市环保科技集团有限公司 | Preparation method and application of aluminum type adsorbent |
| CN115304514A (en) * | 2022-08-17 | 2022-11-08 | 新中天环保股份有限公司 | Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry |
| CN115304514B (en) * | 2022-08-17 | 2023-11-14 | 新中天环保股份有限公司 | Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry |
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