CN106831623B - A method of lead cyanurate is prepared using lead sulfate leachate - Google Patents

A method of lead cyanurate is prepared using lead sulfate leachate Download PDF

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Publication number
CN106831623B
CN106831623B CN201510881260.9A CN201510881260A CN106831623B CN 106831623 B CN106831623 B CN 106831623B CN 201510881260 A CN201510881260 A CN 201510881260A CN 106831623 B CN106831623 B CN 106831623B
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China
Prior art keywords
lead
lead sulfate
leachate
cyanurate
solution
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CN201510881260.9A
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CN106831623A (en
Inventor
曹靖
梁赛
张俊丰
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Xiangtan University
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Xiangtan University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D251/00Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/12Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
    • C07D251/26Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
    • C07D251/30Only oxygen atoms
    • C07D251/32Cyanuric acid; Isocyanuric acid

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention discloses a kind of method using lead sulfate leachate preparation lead cyanurate.Method of the invention be toward lead sulfate leachate in cyanuric acid is first added, add alkali reaction prepare lead cyanurate.The present invention is using the lead sulfate leachate for including from pure lead sulphate or scrap lead or processing obtains, easily prepare the organic lead-salt of high added value, be conducive to recycling for lead resource, have the characteristics that simple process, is swift in response, it is easy to accomplish industrialized production.

Description

A method of lead cyanurate is prepared using lead sulfate leachate
Technical field
The invention belongs to resource reclaim and utilize field, in particular to it is a kind of to prepare lead cyanurate using lead sulfate leachate Method.
Background technique
Lead cyanurate can be used as the heat stabilizer and lubricant of polyvinyl chloride, and there is good lubricity and photo-thermal to stablize Property, it can replace alkali lead sulfate in polyvinyl chloride lead stabilizer, their annual demands reach hundreds of thousands ton.These cyanogen urine There are mainly two types of the preparation methods of lead plumbate, first is that preparation is reacted with cyanuric acid using lead oxide, second is that such as using soluble lead salt The sodium of lead acetate or plumbi nitras and organic matter, sylvite are made.However both methods will be from lead oxide or utilization lead oxide system Standby solubility lead salt starts, this needs to consume a large amount of lead bullion resource, because lead oxide is usually the oxidation system that is milled by lead bullion For what is come out.
Cyanuric acid (English name cyanuric acid) also known as cyanuric acid (tricyanic acid);2,4,6- tri- hydroxyls Base -1,3,5-triazines;2,4,6 trihydroxies-s-triazine (2,4,6-triazinettriol);S-triazine triol (sym- triazinetriol).White crystals are precipitated from water, two crystallizations water of band.Mildly bitter flavor, it is substantially nontoxic, it can be dissolved in hot water, it is micro- It is dissolved in cold water, aqueous solution can be dissolved in the aqueous solution of potassium hydroxide and sodium hydroxide, have insoluble in cold alcohol, ether, benzene etc. in acidity Solvent.Chemical formula is C3H3N3O3, there are two kinds of isomers, i.e. keto-acid and enol-type structure, usually with two kinds of isomers Mixture exist.
Lead resource is a kind of non-renewable resources, and recycling lead resource is a kind of inexorable trend.Have every year a large amount of Scrap lead generate, as lead-acid accumulator it is broken apart go out lead plaster and metallurgy industry in scrap lead slag, however these scrap lead at Divide complexity, it is from a wealth of sources, it is directly unrealistic using scrap lead preparation lead cyanurate and isocyanuric acid lead.But the lead in these scrap lead It is all easy to be transformed into using certain way in more pure lead sulfate, or even many scrap lead and inherently contains a large amount of lead sulfate, Such as lead-acid accumulator it is broken apart go out lead plaster in sulfuric acid lead content up to 50% ~ 70%.Therefore how that lead sulfate is efficient The lead cyanurate that ground is changed into high added value becomes the important topic of lead resource cycle industrial.
Summary of the invention
The present invention provides a kind of method using lead sulfate leachate preparation lead cyanurate.Method of the invention is past sulphur Cyanuric acid is added in lead plumbate leachate, adds alkali reaction and prepares lead cyanurate.
Lead sulfate, which is generally insoluble in water, forms solution, but does not represent it insoluble in other materials.Lead sulfate ammonium salt, Acetate, sodium chloride concentrated solution in have biggish solubility, the feature in these salting liquids can be dissolved in using lead sulfate, Cyanuric acid is added in the leachate of lead sulfate, adds alkali and is convenient to prepare lead cyanurate.
A method of lead cyanurate is prepared using lead sulfate leachate, comprising:
Cyanuric acid is added toward lead sulfate leachate, adds alkali reaction and prepares lead cyanurate.
Further, the lead sulfate refers to wraps in the lead plaster after pure lead sulphate solid or lead-acid accumulator are broken apart The lead sulfate solid for containing or converting;The lead sulfate leachate refer to the lead sulfate be dissolved in the sodium salt of acetic acid, sylvite, ammonium salt or One or more of buffer solution of these salt and acetic acid composition and the solution formed;Or the lead sulfate is dissolved in Sodium chloride, potassium chloride, hydrogen chloride, calcium chloride one or more of solution and the solution that is formed.
Further, the cyanuric acid additional amount and the molar ratio of lead sulfate in leachate are 0.1 ~ 6:1.
Further, the alkali refers to one or more of alkali or alkaline earth metal hydroxide, or is ammonia Water, the molar ratio of lead sulfate is 1 ~ 6:1 in the additional amount and leachate of the alkali.
Further, the reaction, temperature are 0 ~ 120 DEG C, and the time is 0.1~24 hour.
The beneficial effects of the present invention are:
The present invention is easily prepared using the lead sulfate leachate for including from pure lead sulphate or scrap lead or processing obtains The lead cyanurate of high added value out, is conducive to recycling for lead resource, while simple process, being swift in response, it is easy to accomplish work Industry metaplasia produces.
Specific embodiment
The present invention will be further described combined with specific embodiments below, but the present invention is not limited thereto.
Embodiment 1
Lead sulfate leachate is added in stirred tank, the cyanuric acid of 1 times of mole of lead sulfate in solution is added, stirs evenly Afterwards, the potassium hydroxide solid of 3 times of moles of cyanuric acid is added, after 40 DEG C are reacted 2 hours, filters out solid, washing and drying obtains cyanogen urine Lead plumbate solid.The conversion ratio of lead sulfate is 97%, yield 97%.
Embodiment 2
Lead sulfate leachate is added in stirred tank, the cyanuric acid of 0.33 times of mole of lead sulfate in solution is added, stirring is equal After even, the sodium hydrate solid of 3 times of moles of cyanuric acid is added and filters out solid, washing and drying obtains cyanogen after 60 DEG C are reacted 2 hours Uric acid lead solid.The conversion ratio of lead sulfate is 96%, yield 96%.
Embodiment 3
Lead sulfate leachate is added in stirred tank, the cyanuric acid of 0.5 times of mole of lead sulfate in solution is added, stirs evenly Afterwards, the ammonium hydroxide of 3 times of moles of cyanuric acid is added, after 80 DEG C are reacted 5 hours, filters out solid, it is solid to obtain lead cyanurate for washing and drying Body.The conversion ratio of lead sulfate is 95%, yield 95%.

Claims (1)

1. a kind of method using lead sulfate leachate preparation lead cyanurate, comprising: cyanuric acid is added toward lead sulfate leachate, then Alkali is added, at a temperature of 0~120 DEG C, reacts 0.1~24 hour, prepares lead cyanurate, the additional amount and leachate of cyanuric acid The molar ratio of middle lead sulfate is 0.1~6: 1;
The lead sulfate, which refers in the lead plaster after pure lead sulphate solid or lead-acid accumulator are broken apart, includes or the sulphur of conversion Lead plumbate solid;The lead sulfate leachate refer to the lead sulfate be dissolved in the solution that the sodium salt, sylvite, ammonium salt of acetic acid are formed or One or more of buffer solution of these salt and acetic acid composition and the solution formed;Or the lead sulfate is dissolved in Sodium chloride, potassium chloride, hydrogen chloride, calcium chloride one or more of solution and the solution that is formed;
The alkali refers to one or more of alkali or alkaline earth metal hydroxide, or is ammonium hydroxide, and the alkali adds The molar ratio for entering lead sulfate in amount and leachate is 1-6: 1.
CN201510881260.9A 2015-12-07 2015-12-07 A method of lead cyanurate is prepared using lead sulfate leachate Expired - Fee Related CN106831623B (en)

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Publication number Priority date Publication date Assignee Title
CN107383430A (en) * 2017-07-31 2017-11-24 马鞍山市瑞鹏科技有限公司 A kind of lead cyanurate composite stabilizer production system and its processing method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101463142A (en) * 2008-12-29 2009-06-24 南京协和化学有限公司 Production process of lead cyanurate composite stabilizer
CN104762480A (en) * 2015-04-24 2015-07-08 南京环宏资源再生科技有限公司 Method for recovering lead from waste lead storage battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101463142A (en) * 2008-12-29 2009-06-24 南京协和化学有限公司 Production process of lead cyanurate composite stabilizer
CN104762480A (en) * 2015-04-24 2015-07-08 南京环宏资源再生科技有限公司 Method for recovering lead from waste lead storage battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
难处理铅锌矿酸浸渣回收硫酸铅的工艺研究;张传宝等;《应用化工》;20170731;第41卷(第7期);1188-1192

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