CN107311950A - A kind of preparation method of cyanuric acid lanthanum - Google Patents
A kind of preparation method of cyanuric acid lanthanum Download PDFInfo
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- CN107311950A CN107311950A CN201710643402.7A CN201710643402A CN107311950A CN 107311950 A CN107311950 A CN 107311950A CN 201710643402 A CN201710643402 A CN 201710643402A CN 107311950 A CN107311950 A CN 107311950A
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- cyanuric acid
- water
- lanthanum
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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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- Organic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation method of cyanuric acid lanthanum, comprise the following steps：A. water and cyanuric acid are proportionally added into reactor, 60~80 DEG C is heated under then stirring, treats that cyanuric acid is dissolved completely in water, cyanuric acid solution for later use is formed；B. before step a is carried out or while carrying out step a, water, lanthana are got out in proportion, ready lanthana is added in ready water suspension is made；C. suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted, temperature is progressively risen to 80~85 DEG C when being reacted；D. treat to cool the temperature to 10~30 DEG C after the completion of the reaction in step c, the reaction solution that reaction is obtained is filtered, washed, dried and crushed, and finally gives cyanuric acid lanthanum.The problem of existing production cyanuric acid lanthanum solved can produce brine waste.
Description
Technical field
The present invention relates to chemical field, and in particular to a kind of preparation method of cyanuric acid lanthanum.
Background technology
Existing cyanuric acid lanthanum is Material synthesis generally by cyanuric acid, lanthanum nitrate, sodium hydroxide, but the side as
Method can produce brine waste to manufacture cyanuric acid lanthanum, and cost is also higher.
The content of the invention
It is an object of the invention to provide a kind of preparation method of cyanuric acid lanthanum, the existing production cyanuric acid lanthanum of solution can be produced
The problem of raw brine waste.
To solve above-mentioned technical problem, the present invention uses following technical scheme：
A kind of preparation method of cyanuric acid lanthanum, comprises the following steps：A. water and cyanuric acid are proportionally added into reactor, then
60~80 DEG C are heated under stirring, treats that cyanuric acid is dissolved completely in water, cyanuric acid solution for later use is formed；B. step a is being carried out
Before or while carry out step a, water, lanthana are got out in proportion, ready lanthana is added in ready water
Suspension is made；C. suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted, will when being reacted
Temperature progressively rises to 80~85 DEG C；D. treat to cool the temperature to 10~30 DEG C after the completion of the reaction in step c, by react obtain it is anti-
Answer liquid to be filtered, wash, drying and crushing, finally giving cyanuric acid lanthanum.
Present invention employs the oxide of lanthanum or hydroxide, the new side of cyanuric acid lanthanum is prepared without the inorganic salts using lanthanum
Method, because cyanuric acid solubility in cold water is small, it is therefore desirable to heated in dissolving, by suspension slow adding at the uniform velocity
When entering into cyanuric acid solution, maintain the temperature at more than 60 DEG C, when cyanuric acid and lanthana react, by temperature by
Step rises to 80~85 DEG C, because cyanuric acid is a kind of complicated compound, if temperature directly is raised into highest at the very start, instead
Various accessory substances excessively acutely should can be generated, influence the purity of cyanuric acid lanthanum, and temperature is stepped up to reduce accessory substance
Production, brine waste, non-wastewater discharge will not be produced by carrying out production using said new method, and production cost is relatively low.
As present invention further optimization, the mass fraction of above-mentioned steps a reclaimed waters and cyanuric acid is respectively 6~12 parts of water
With 3~5 parts of cyanuric acid.
It is in order that cyanuric acid is dissolved completely in water that water and cyanuric acid carry out preparation by said ratio.
As present invention further optimization, the mass fraction of above-mentioned steps b reclaimed waters and lanthana be respectively 3~5 parts of water,
1~1.5 part of lanthana.
As present invention further optimization, the mass fraction of suspension and cyanuric acid solution in above-mentioned steps c is distinguished
For 4~6.5 parts of suspension, 9~17 parts of cyanuric acid solution.
Said ratio is prepared according to the amount that the lanthana in cyanuric acid and suspension is dissolved in water, can fill it
Point reaction, it is to avoid cause the waste of raw material, cyanuric acid is three hydroxyls, lanthanum ion trivalent, by 1 part of cyanuric acid of mass fraction and
1.26 parts of lanthana reacteds just, and in above-mentioned course of reaction cyanuric acid excess three times more than, i.e., 3 ~ 5 parts cyanuric acids and 1.26
Part lanthana reacted, more than 3 parts are excessive, may loop to next dispensing, so react, can obtain a centre
For lanthanum atom, three angles are the product of cyanuric acid structure.
As present invention further optimization, the time persistently reacted in above-mentioned steps c is 1~3 hour.
Sustained response 1~3 hour is to react more abundant to allow, it is to avoid cause the waste of raw material.
As present invention further optimization, the liquid that will be obtained in above-mentioned steps d after reacting liquid filtering is directly used in molten
Solve cyanuric acid or for formulated suspension, recycled.
Because will obtain also containing cyanuric acid in liquid after reacting liquid filtering, therefore it can be directly used for dissolving cyanuric acid or use
In formulated suspension, recycled, it is to avoid cause to waste, reduce production cost.
A kind of preparation method of cyanuric acid lanthanum, comprises the following steps：（1）Water and cyanogen urine are proportionally added into reactor
Acid, is heated to 60~80 DEG C under then stirring, treats that cyanuric acid is dissolved completely in water, forms cyanuric acid solution for later use；（2）Exist
Before carrying out step a or while carrying out step a, water, lanthanum hydroxide are got out in proportion, ready lanthanum hydroxide is added
Suspension is made in ready water；（3）Suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted,
Temperature is progressively risen to 80~85 DEG C when being reacted；（4）Treat to cool the temperature to 10~30 after the completion of the reaction in step c
DEG C, the reaction solution that reaction is obtained is filtered, washed, being dried and being crushed, and finally gives cyanuric acid lanthanum, the step（2）In
The quality for adding lanthanum hydroxide is 1.116 times of lanthana consumption in above-mentioned steps b.
Compared with prior art, the beneficial effects of the invention are as follows：
1. production will not produce brine waste, non-wastewater discharge, and production cost is relatively low.
2. simple production process, it is easy to promote.
3. raw material can be utilized sufficiently, waste can be reduced.
4. the accessory substance of generation is few, the cyanuric acid lanthanum produced is more pure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Specific embodiment 1
A kind of preparation method of cyanuric acid lanthanum, comprises the following steps：：A. water and cyanuric acid are proportionally added into reactor, so
60~80 DEG C are heated under stirring afterwards, treats that cyanuric acid is dissolved completely in water, cyanuric acid solution for later use is formed；B. step is being carried out
Before a or while carrying out step a, water, lanthana are got out in proportion, and ready lanthana is added in ready water
Suspension is made；C. suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted, will when being reacted
Temperature progressively rises to 80~85 DEG C；D. treat to cool the temperature to 10~30 DEG C after the completion of the reaction in step c, by react obtain it is anti-
Answer liquid to be filtered, wash, drying and crushing, finally giving cyanuric acid lanthanum.
Present invention employs the oxide of lanthanum or hydroxide, the new side of cyanuric acid lanthanum is prepared without the inorganic salts using lanthanum
Method, because cyanuric acid solubility in cold water is small, it is therefore desirable to heated in dissolving, by suspension slow adding at the uniform velocity
When entering into cyanuric acid solution, maintain the temperature at more than 60 DEG C, when cyanuric acid and lanthana react, by temperature by
Step rises to 80~85 DEG C, because cyanuric acid is a kind of complicated compound, if temperature directly is raised into highest at the very start, instead
Various accessory substances excessively acutely should can be generated, influence the purity of cyanuric acid lanthanum, and temperature is stepped up to reduce accessory substance
Production, brine waste, non-wastewater discharge will not be produced by carrying out production using said new method, and production cost is relatively low.
Specific embodiment 2：
The present embodiment is that the mass fraction of step a reclaimed waters and cyanuric acid has been carried out further on the basis of specific embodiment 1
Explanation, the mass fraction of above-mentioned steps a reclaimed waters and cyanuric acid is respectively 3~5 parts of 6~12 parts of water and cyanuric acid.
It is in order that cyanuric acid is dissolved completely in water that water and cyanuric acid carry out preparation by said ratio.
Specific embodiment 3：
The present embodiment is that the mass fraction of step a reclaimed waters and cyanuric acid has been carried out further on the basis of specific embodiment 2
Explanation, the mass fraction of above-mentioned steps a reclaimed waters and cyanuric acid is respectively 3 parts of 6 parts of water and cyanuric acid.
Specific embodiment 4：
The present embodiment is that the mass fraction of step a reclaimed waters and cyanuric acid has been carried out further on the basis of specific embodiment 2
Explanation, the mass fraction of above-mentioned steps a reclaimed waters and cyanuric acid is respectively 4 parts of 10 parts of water and cyanuric acid.
Specific embodiment 5：
The present embodiment is that the mass fraction of step a reclaimed waters and cyanuric acid has been carried out further on the basis of specific embodiment 2
Explanation, the mass fraction of above-mentioned steps a reclaimed waters and cyanuric acid is respectively 5 parts of 12 parts of water and cyanuric acid.
Specific embodiment 6：
The present embodiment is that the mass fraction of step b reclaimed waters and lanthana has been carried out further on the basis of specific embodiment 1
Explanation, the mass fraction of above-mentioned steps b reclaimed waters and lanthana is respectively 3~5 parts of water, 1~1.5 part of lanthana.
Specific embodiment 7：
The present embodiment is that the mass fraction of step b reclaimed waters and lanthana has been carried out further on the basis of specific embodiment 6
Explanation, the mass fraction of above-mentioned steps b reclaimed waters and lanthana is respectively 3 parts of water, 1 part of lanthana.
Specific embodiment 8：
The present embodiment is that the mass fraction of step b reclaimed waters and lanthana has been carried out further on the basis of specific embodiment 6
Explanation, the mass fraction of above-mentioned steps b reclaimed waters and lanthana is respectively 3.8 parts of water, 1.4 parts of lanthana.
Specific embodiment 9：
The present embodiment is that the mass fraction of step b reclaimed waters and lanthana has been carried out further on the basis of specific embodiment 6
Explanation, the mass fraction of above-mentioned steps b reclaimed waters and lanthana is respectively 5 parts of water, 1.5 parts of lanthana.
Specific embodiment 10：
The present embodiment is that the mass fraction of suspension and cyanuric acid solution in step c is carried out on the basis of specific embodiment 1
The mass fraction of suspension and cyanuric acid solution in further instruction, above-mentioned steps c is respectively 4~6.5 parts of suspension, cyanogen
9~17 parts of uric acid solution.
Said ratio is prepared according to the amount that the lanthana in cyanuric acid and suspension is dissolved in water, can fill it
Point reaction, it is to avoid cause the waste of raw material, cyanuric acid is three hydroxyls, lanthanum ion trivalent, by 1 part of cyanuric acid of mass fraction and
1.26 parts of lanthana reacteds just, and in above-mentioned course of reaction cyanuric acid excess three times more than, i.e., 3 ~ 5 parts cyanuric acids and 1.26
Part lanthana reacted, more than 3 parts are excessive, may loop to next dispensing, so react, can obtain a centre
For lanthanum atom, three angles are the product of cyanuric acid structure.
Specific embodiment 11：
The present embodiment is that the mass fraction of suspension and cyanuric acid solution in step c is carried out on the basis of specific embodiment 10
The mass fraction of suspension and cyanuric acid solution in further instruction, above-mentioned steps c is respectively 4 parts of suspension, cyanogen urine
9 parts of acid solution.
Specific embodiment 12：
The present embodiment is that the mass fraction of suspension and cyanuric acid solution in step c is carried out on the basis of specific embodiment 10
The mass fraction of suspension and cyanuric acid solution in further instruction, above-mentioned steps c is respectively 5 parts of suspension, cyanogen urine
15 parts of acid solution.
Specific embodiment 13：
The present embodiment is that the mass fraction of suspension and cyanuric acid solution in step c is carried out on the basis of specific embodiment 10
The mass fraction of suspension and cyanuric acid solution in further instruction, above-mentioned steps c is respectively 6.5 parts of suspension, cyanogen
17 parts of uric acid solution.
Specific embodiment 14：
The present embodiment is that the time persistently reacted in step c has been carried out further on the basis of specific embodiment 1
Illustrate, the time persistently reacted in above-mentioned steps c is 1~3 hour.
Sustained response 1~3 hour is to react more abundant to allow, it is to avoid cause the waste of raw material.
Specific embodiment 15：
The present embodiment is that the liquid obtained after being filtered on the basis of specific embodiment 1 to step d has carried out further instruction,
The liquid that will be obtained in above-mentioned steps d after reacting liquid filtering, is directly used in dissolving cyanuric acid or for formulated suspension, is followed
Ring is utilized.
Because will obtain also containing cyanuric acid in liquid after reacting liquid filtering, therefore it can be directly used for dissolving cyanuric acid or use
In formulated suspension, recycled, it is to avoid cause to waste, reduce production cost.
Specific embodiment 16：
A kind of preparation method of cyanuric acid lanthanum, comprises the following steps：（1）Water and cyanuric acid are proportionally added into reactor, so
60~80 DEG C are heated under stirring afterwards, treats that cyanuric acid is dissolved completely in water, cyanuric acid solution for later use is formed；（2）Walked
Before rapid a or while carrying out step a, water, lanthanum hydroxide are got out in proportion, and ready lanthanum hydroxide is added and is ready to
Water in suspension is made；（3）Suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted, carried out
Temperature is progressively risen to 80~85 DEG C during reaction；（4）Treat to cool the temperature to 10~30 DEG C after the completion of the reaction in step c, will be anti-
The reaction solution that should be obtained is filtered, washed, being dried and being crushed, and finally gives cyanuric acid lanthanum, the step（2）Middle addition hydrogen-oxygen
The quality for changing lanthanum is 1.116 times of lanthana consumption in above-mentioned steps b.
Although reference be made herein to invention has been described for multiple explanatory embodiments of the invention, however, it is to be understood that
Those skilled in the art can be designed that a lot of other modification and embodiment, and these modifications and embodiment will fall in this Shen
Please be within disclosed spirit and spirit.More specifically, can be to master in the range of disclosure and claim
The building block and/or layout for inscribing composite configuration carry out a variety of variations and modifications.Except what is carried out to building block and/or layout
Outside modification and improvement, to those skilled in the art, other purposes also will be apparent.
Claims (7)
1. a kind of preparation method of cyanuric acid lanthanum, it is characterised in that：Comprise the following steps：A. water is proportionally added into reactor
And cyanuric acid, 60-80 DEG C is heated under then stirring, treats that cyanuric acid is dissolved completely in water, cyanuric acid solution for later use is formed；b.
Before step a is carried out or while carrying out step a, water, lanthana are got out in proportion, ready lanthana are added accurate
Suspension is made in the water got ready；C. suspension is at the uniform velocity added in cyanuric acid solution, both is persistently reacted, entered
Temperature is progressively risen to 80-85 DEG C during row reaction；D. treat to cool the temperature to 10-30 DEG C after the completion of the reaction in step c, will react
Obtained reaction solution is filtered, washed, being dried and being crushed, and finally gives cyanuric acid lanthanum.
2. a kind of preparation method of cyanuric acid lanthanum according to claim 1, it is characterised in that：The step a reclaimed waters and cyanogen
The mass fraction of uric acid is respectively 3-5 parts of 6-12 parts of water and cyanuric acid.
3. a kind of preparation method of cyanuric acid lanthanum according to claim 1, it is characterised in that：The step b reclaimed waters and oxygen
The mass fraction for changing lanthanum is respectively 3-5 parts of water, 1-1.5 parts of lanthana.
4. a kind of preparation method of cyanuric acid lanthanum according to claim 1, it is characterised in that：Suspension in the step c
The mass fraction of liquid and cyanuric acid solution is respectively 4-6.5 parts of suspension, 9-17 parts of cyanuric acid solution.
5. a kind of preparation method of cyanuric acid lanthanum according to claim 1, it is characterised in that：Persistently sent out in the step c
The time of raw reaction is 1-3 hours.
6. a kind of preparation method of cyanuric acid lanthanum according to claim 1, it is characterised in that：Will reaction in the step d
The liquid obtained after liquid filtering, is directly used in dissolving cyanuric acid or for formulated suspension, is recycled.
7. a kind of preparation method of cyanuric acid lanthanum, it is characterised in that：Comprise the following steps：（1）It is proportionally added into reactor
Water and cyanuric acid, are heated to 60-80 DEG C under then stirring, treat that cyanuric acid is dissolved completely in water, form cyanuric acid solution for later use；
（2）Before step a is carried out or while carrying out step a, water, lanthanum hydroxide are got out in proportion, by ready hydroxide
Lanthanum adds in ready water and suspension is made；（3）Suspension is at the uniform velocity added in cyanuric acid solution, both is persistently sent out
Raw reaction, 80-85 DEG C is progressively risen to when being reacted by temperature；（4）Treat to cool the temperature to after the completion of the reaction in step c
10-30 DEG C, the reaction solution that reaction is obtained is filtered, washed, being dried and being crushed, and finally gives cyanuric acid lanthanum, the step
（2）The quality of middle addition lanthanum hydroxide is 1.116 times of lanthana consumption in claim 1 step b.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710643402.7A CN107311950A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of cyanuric acid lanthanum |
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| CN201710643402.7A CN107311950A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of cyanuric acid lanthanum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108912542A (en) * | 2018-06-26 | 2018-11-30 | 河南省化工研究所有限责任公司 | A kind of calcium-zinc composite stabilizing agent and preparation method thereof that environment-friendly type is rare earth modified |
| CN111934015A (en) * | 2020-08-28 | 2020-11-13 | 珠海市赛纬电子材料股份有限公司 | Non-aqueous electrolyte of lithium ion battery and lithium ion battery containing non-aqueous electrolyte |
-
2017
- 2017-07-31 CN CN201710643402.7A patent/CN107311950A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108912542A (en) * | 2018-06-26 | 2018-11-30 | 河南省化工研究所有限责任公司 | A kind of calcium-zinc composite stabilizing agent and preparation method thereof that environment-friendly type is rare earth modified |
| CN111934015A (en) * | 2020-08-28 | 2020-11-13 | 珠海市赛纬电子材料股份有限公司 | Non-aqueous electrolyte of lithium ion battery and lithium ion battery containing non-aqueous electrolyte |
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