CN105524005B - A method of recycling cyanuric acid from cyanuric acid waste residue - Google Patents
A method of recycling cyanuric acid from cyanuric acid waste residue Download PDFInfo
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- CN105524005B CN105524005B CN201510970701.2A CN201510970701A CN105524005B CN 105524005 B CN105524005 B CN 105524005B CN 201510970701 A CN201510970701 A CN 201510970701A CN 105524005 B CN105524005 B CN 105524005B
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- cyanuric acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic 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
- C07D251/26—Heterocyclic 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
- C07D251/30—Only oxygen atoms
- C07D251/32—Cyanuric acid; Isocyanuric acid
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Abstract
The method that the invention discloses a kind of to recycle cyanuric acid from cyanuric acid waste residue, belongs to environmental technology field.This method mixes specifically includes the following steps: water and cyanuric acid waste residue are consolidated mass ratio with the liquid of 2~5:1,10~25min of heating hydrolysis at 105~155 DEG C；Decolorising agent is added in feed liquid with the solid-liquid mass ratio of 0.01~0.05:1, is filtered after stirring 15~45min；Filtrate is taken, at 10~30 DEG C after cooling 3~6h, cyanuric acid crude product is obtained by filtration again；Obtained cyanuric acid crude product after dry 4~7h, is obtained into high-purity cyanuric acid at 80~110 DEG C.The obtained cyanuric acid product color of the present invention is white, purity and high income.Especially prepared decolorising agent, decolorizing efficiency are high, reusable.
Description
Technical field
The invention belongs to environmental technology fields, and in particular to the utilization of solid slag, more particularly to it is a kind of from trimerization
The method of cyanuric acid is recycled in cyanic acid waste residue.
Background technique
Cyanuric acid (also referred to as cyanuric acid) is a kind of important industrial chemicals, is mainly used for synthesizing new bleaching agent, antioxygen
Agent, paint, agriculture herbicide and metal cyanide corrosion inhibiter.It can be used for swimming pool chlorine stabilizer, can also be used for sterilizing, go
It is dirty；It also can be directly used for nylon, Sai Ke, fire retardant and cosmetic additive agent etc..
Currently, using sym-closene during the key intermediate five-carbon ring aldehydo of isoprene method synthesis vitamin A
As chlorohydrination reagent, sym-closene produces a large amount of by-product cyanuric acid waste residue during the reaction, main
Ingredient is cyanuric acid, chloro isonitrile uric acid (trichlorine isonitrile uric acid, isocyanide dichloride uric acid, a chlorine isonitrile uric acid), other impurity
Deng.If do not recycled, not only pollute the environment, and improves product cost.Patent CN1844077A is by that will react
The cyanuric acid waste residue generated in the process is directly cleaned with water or methanol or acetone, obtains pulverulent solids cyanuric acid.But
Cyanuric acid not white color, the purity recycled using this method is not high, it is difficult to directly reuse.
Summary of the invention
In order to overcome the deficiencies of the prior art, the purpose of the present invention is to provide one kind recycles trimerization from cyanuric acid waste residue
The method of cyanic acid, to obtain white color, purity is high, the cyanuric acid that can directly reuse.
In order to achieve the above technical purposes, the present invention is achieved by the following technical programs.
The method that the present invention provides a kind of to recycle cyanuric acid from cyanuric acid waste residue, including following operating procedure:
Water and cyanuric acid waste residue are consolidated mass ratio with the liquid of 2~5:1 to mix, the heating hydrolysis 10 at 105~155 DEG C
~25min；Decolorising agent is added in feed liquid with the solid-liquid mass ratio of 0.01~0.05:1, is filtered after stirring 15~45min；Take filter
Cyanuric acid crude product is obtained by filtration at 10~30 DEG C after cooling 3~6h in liquid again；By obtained cyanuric acid crude product 80
At~110 DEG C after dry 4~7h, high-purity cyanuric acid is obtained；
The decolorising agent is one of active carbon from coal, wood activated charcoal and cocoanut active charcoal, and with Mn (NO3)2、
NH4VO3、ZrOCl2·8H2One of O solution impregnates 12 at 60~90 DEG C~for 24 hours, then in 400~700 DEG C of nitrogen atmosphere
3~6h of middle roasting and obtain.
Preferably, the water and cyanuric acid waste residue are consolidated mass ratio with the liquid of 3~4:1 and are mixed, and add at 120~140 DEG C
15~20min of pyrohydrolysis.
Preferably, the dipping temperature of the decolorising agent is 70~80 DEG C, and dip time is 15~20h, maturing temperature 450
~650 DEG C, calcining time is 4~5h.
Preferably, the solid-liquid mass ratio of the decolorising agent and feed liquid be 0.03~0.05:1, mixing time be 30~
40min。
Preferably, the filtrate cooling 4~5.5h at 20~28 DEG C, filtered cyanuric acid crude product is 95 again
~105 DEG C of dry 5.5~6.5h.
The principles of science of the invention is as follows:
The present invention is added bleaching agent bleaching, through supercooling, crystallization after filtering, obtains by hydrolyzing cyanuric acid waste residue
High-purity cyanuric acid product.By the way of the hydrolysis of cyanuric acid waste residue, chloro isonitrile uric acid can be made to be completely converted into three
Paracyanogen acid, obtained cyanuric acid product colour is pure white, and the purity and yield of cyanuric acid are respectively up to 99.33% He
94.12%.Chloro isonitrile uric acid hydrolysis principle in cyanuric acid waste residue is shown below.
Compared with prior art, the present invention has following technical effect that
1, the decolorising agent prepared by the present invention, decolorizing efficiency is high, and reusing is good.
2, for the present invention using the method for hydrolysis, decoloration, technical process is simple, and production cost is low, considerably increases production exercise
The feasibility of work.
3, the obtained cyanuric acid product color of the present invention is white, purity and high income.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
(1) wood activated charcoal is cleaned with the HCl solution that molar concentration is 0.01mol/L, is washed with deionized water after suction filtration
It washs to neutrality, is dried under the conditions of 80 DEG C.
(2) 250mL is placed in water-bath with the three-necked flask of thermometer, it is 0.5mol/L's that 50mL molar concentration, which is added,
Mn(NO3)2Solution and 10g pass through pretreated wood activated charcoal.Keep the temperature 60 DEG C of stirred in water bath.After 12h, filtering is gone with 15mL
Then ion water washing dries 5h at a temperature of 90 DEG C.
(3) the wood activated charcoal 9g obtained is put in pipe reaction furnace in nitrogen atmosphere and roasts at 400 DEG C, constant temperature 3h
Afterwards, decolorising agent is obtained.
(4) 100mL deionized water and 50g trimerization is added with being placed in oil bath in the three-necked flask of thermometer in 500mL
Cyanic acid waste residue.It keeps the temperature after stirring 10min in 105 DEG C of oil baths, decolorising agent 7.5g is added, after stirring 15min, be separated by filtration active carbon
Solid slag obtains filtrate.
(5) cyanuric acid crude product is obtained by filtration after 10 DEG C of cooling 3h in obtained filtrate, and dry 4h, obtains at 80 DEG C
To high-purity cyanuric acid.Cyanuric acid purity is 91.23%, yield 82.31%, and filtrate percent of decolourization is 73.62%.
Embodiment 2
(1) active carbon from coal is cleaned with the HCl solution that molar concentration is 0.01mol/L, is washed with deionized water after suction filtration
It washs to neutrality, is dried under the conditions of 80 DEG C.
(2) 250mL is placed in water-bath with the three-necked flask of thermometer, it is 0.5mol/L's that 50mL molar concentration, which is added,
NH4VO3Solution and the pretreated 10g active carbon from coal of process.Keep the temperature 80 DEG C of stirred in water bath.After 18h, filtering, with 15mL go from
Then sub- water washing dries 5h at a temperature of 90 DEG C.
(3) the active carbon from coal 9g obtained is put in pipe reaction furnace in nitrogen atmosphere and roasts at 550 DEG C, constant temperature 4h
Afterwards, decolorising agent is obtained.
(4) 150mL deionized water and 50g trimerization is added with being placed in oil bath in the three-necked flask of thermometer in 500mL
Cyanic acid waste residue.It keeps the temperature after stirring 20min in 120 DEG C of oil baths, decolorising agent 4g is added, after stirring 35min, it is solid to be separated by filtration active carbon
Slag obtains filtrate.
(5) cyanuric acid crude product is obtained by filtration after 15 DEG C of cooling 4h in obtained filtrate, and dry 5h, obtains at 90 DEG C
To high-purity cyanuric acid.Cyanuric acid purity is 94.27%, yield 87.23%, and filtrate percent of decolourization is 78.46%.
Embodiment 3
(1) cocoanut active charcoal is cleaned with the HCl solution that molar concentration is 0.01mol/L, is washed with deionized water after suction filtration
It washs to neutrality, is dried under the conditions of 80 DEG C.
(2) 250mL is placed in water-bath with the three-necked flask of thermometer, addition 50mL molar concentration is 0.5mol/L
ZrOCl2·8H2O solution and the pretreated 10g cocoanut active charcoal of process.Keep the temperature 90 DEG C of stirred in water bath.After for 24 hours, filtering is used
The washing of 15mL deionized water, then dries 5h at a temperature of 90 DEG C.
(3) the cocoanut active charcoal 9g obtained is put in pipe reaction furnace in nitrogen atmosphere and roasts at 700 DEG C, constant temperature 6h
Afterwards, decolorising agent is obtained.
(4) 250mL deionized water and 50g trimerization is added with being placed in oil bath in the three-necked flask of thermometer in 500mL
Cyanic acid waste residue.It keeps the temperature after stirring 25min in 155 DEG C of oil baths, decolorising agent 3g is added, after stirring 45min, it is solid to be separated by filtration active carbon
Slag obtains filtrate.
(5) cyanuric acid crude product is obtained by filtration after 30 DEG C of cooling 6h in obtained filtrate, and dry 7h, obtains at 110 DEG C
To high-purity cyanuric acid.Cyanuric acid purity is 89.88%, yield 79.23%, and filtrate percent of decolourization is 74.83%.
Embodiment 4
(1) active carbon from coal is cleaned with the HCl solution that molar concentration is 0.01mol/L, is washed with deionized water after suction filtration
It washs to neutrality, is dried under the conditions of 80 DEG C.
(2) 250mL is placed in water-bath with the three-necked flask of thermometer, it is 0.5mol/L's that 50mL molar concentration, which is added,
ZrOCl2·8H2O solution and the pretreated 10g active carbon from coal of process.Keep the temperature 75 DEG C of stirred in water bath.After 18h, filtering is used
The washing of 15mL deionized water, then dries 5h at a temperature of 90 DEG C.
(3) the active carbon from coal 6g obtained is put in pipe reaction furnace in nitrogen atmosphere and roasts at 500 DEG C, constant temperature
After 4.5h, decolorising agent is obtained.
(4) 175mL deionized water and 50g trimerization is added with being placed in oil bath in the three-necked flask of thermometer in 500mL
Cyanic acid waste residue.It keeps the temperature after stirring 17min in 130 DEG C of oil baths, decolorising agent 9g is added, after stirring 35min, it is solid to be separated by filtration active carbon
Slag obtains filtrate.
(5) cyanuric acid crude product is obtained by filtration after 25 DEG C of cooling 5h in obtained filtrate, and dry 6h, obtains at 100 DEG C
To high-purity cyanuric acid.Cyanuric acid purity is 99.33%, yield 92.34%, and filtrate percent of decolourization is 81.24%.
Claims (1)
1. a kind of method for recycling cyanuric acid from cyanuric acid waste residue, it is characterised in that the following steps are included:
(1) active carbon from coal is cleaned with the HCl solution that molar concentration is 0.01mol/L, be washed with deionized after suction filtration to
Neutrality is dried under the conditions of 80 DEG C；
(2) 250mL is placed in water-bath with the three-necked flask of thermometer, it is 0.5mol/L's that 50mL molar concentration, which is added,
ZrOCl2·8H2O solution and pass through pretreated 10g active carbon from coal, keeps the temperature 75 DEG C of stirred in water bath, after 18h, filtering is used
The washing of 15mL deionized water, then dries 5h at a temperature of 90 DEG C；
(3) the active carbon from coal 6g obtained is put in pipe reaction furnace in nitrogen atmosphere and roasts at 500 DEG C, after constant temperature 4.5h,
Obtain decolorising agent；
(4) 175mL deionized water and 50g cyanuric acid is added with being placed in oil bath in the three-necked flask of thermometer in 500mL
Waste residue is kept the temperature after stirring 17min in 130 DEG C of oil baths, and decolorising agent 9g is added, and after stirring 35min, is separated by filtration active carbon solid slag and is obtained
To filtrate；
(5) cyanuric acid crude product is obtained by filtration after 25 DEG C of cooling 5h in obtained filtrate, and dry 6h, obtains height at 100 DEG C
Purity cyanuric acid.
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Citations (5)
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|---|---|---|---|---|
| CN1394820A (en) * | 2001-11-23 | 2003-02-05 | 广西南宁科林特技术工程有限公司 | Method for treating waste water produced by chloro-isocyanuric acid production |
| CN1844077A (en) * | 2006-05-17 | 2006-10-11 | 绍兴文理学院 | Method for preparing 1-chloro-2-methyl-4-alkylacyloxy-2-butene |
| CN101323795A (en) * | 2008-07-15 | 2008-12-17 | 西南石油大学 | Preparation of gasoline desulphurization sorbent |
| CN101878435A (en) * | 2007-09-28 | 2010-11-03 | 莫弗探测公司 | Systems and methods for reducing false alarms in detection systems |
| CN103182243A (en) * | 2013-03-25 | 2013-07-03 | 江苏中材环境工程有限公司 | Preparation and application method of smoke denitrifying agent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5599380A (en) * | 1979-01-25 | 1980-07-29 | Shikoku Chem Corp | Treating method for waste liquid of aqueous solution containing cyanuric acid |
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2015
- 2015-12-21 CN CN201510970701.2A patent/CN105524005B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394820A (en) * | 2001-11-23 | 2003-02-05 | 广西南宁科林特技术工程有限公司 | Method for treating waste water produced by chloro-isocyanuric acid production |
| CN1844077A (en) * | 2006-05-17 | 2006-10-11 | 绍兴文理学院 | Method for preparing 1-chloro-2-methyl-4-alkylacyloxy-2-butene |
| CN101878435A (en) * | 2007-09-28 | 2010-11-03 | 莫弗探测公司 | Systems and methods for reducing false alarms in detection systems |
| CN101323795A (en) * | 2008-07-15 | 2008-12-17 | 西南石油大学 | Preparation of gasoline desulphurization sorbent |
| CN103182243A (en) * | 2013-03-25 | 2013-07-03 | 江苏中材环境工程有限公司 | Preparation and application method of smoke denitrifying agent |
Non-Patent Citations (2)
| Title |
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| 三聚氰氯和它的合成;成都工学院化工系有机化学教研组;《化学世界》;19590131;全文 |
| 氰尿酸合成研究的进展;裘兆蓉，等;《江苏石油化工学院学报》;19990331;第11卷(第1期);全文 |
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