CN106810470A - A kind of preparation technology of guanidine nitrate - Google Patents
A kind of preparation technology of guanidine nitrate Download PDFInfo
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- CN106810470A CN106810470A CN201510852889.0A CN201510852889A CN106810470A CN 106810470 A CN106810470 A CN 106810470A CN 201510852889 A CN201510852889 A CN 201510852889A CN 106810470 A CN106810470 A CN 106810470A
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- China
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- preparation technology
- reaction
- guanidine nitrate
- nitrate
- steel ball
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/02—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of guanidine from cyanamide, calcium cyanamide or dicyandiamides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation technology of guanidine nitrate, to adding thin steel ball in reaction mass dicyandiamide and ammonium nitrate, by the collision of steel ball, grinding material in stirring reaction, it is achieved thereby that material is more fully contacted and reacts, have effectively achieved and promote reaction forward to carry out and at utmost avoid the purpose of side reaction, and then impurity content is few in causing product, product purity is improved, the production in enormous quantities of guanidine nitrate high-purity is enabled, with extensive industrial value and market prospects.
Description
Technical field
The present invention relates to a kind of preparation technology of guanidine nitrate, belong to organic synthesis field.
Background technology
Guanidine compound has a wide range of applications in fields such as medicine, fine chemistry industries.Guanidine nitrate, also known as two
Amino-guanidine nitrate, is a kind of important chemical and medicine industry intermediate, and for example it can be phonetic as sulphoamidine, sulfanilamide (SN)
The intermediate of the medicines such as pyridine, also can be used as the chemical intermediate of other guanidinesalts (such as guanidine carbonate).Its tradition
Synthetic method has：(1) prepared using dicyandiamide and ammonium nitrate frit reaction, (2) are urinated using molten state
Element and ammonium nitrate generate guanidine nitrate and aminoquinoxaline under catalyst action, but these traditional handicrafts due to
The unreasonable and guanidine nitrate that be often difficult to prepare high-purity of processing step or condition, so that numerous
Trivial post processing purification step, so as to increased the application that production cost limits its large-scale production.
For many defects of prior art, the present inventor is intended to develop a kind of guanidine nitrate preparation work of novelty
Skill, by the optimization of processing step and condition realize in high yield, high-purity prepare target product, meet
The use demand of chemical industry, medicine and other fields.
The content of the invention
For above-mentioned many defects, the present inventor fills by substantial amounts of further investigation having paid
After the creative work for dividing, a kind of new guanidine nitrate preparation technology is have developed, so as to complete the present invention.
The present invention relates to a kind of preparation technology of guanidine nitrate, its concrete technology step is as follows：
(1) ammonium nitrate is crushed, crosses 70 mesh sieves, the ammonium nitrate fine powder for sifting out is standby；
(2) by ammonium nitrate fine powder and dicyandiamide with 2:1 is matched, and mixes a diameter of 8mm thereto
Thin steel ball, is well mixed, wherein dicyandiamide quality:The number of steel ball is 100:1g/；
(3) divide 3 batches to complete charging, be placed in reactor, controlling reaction temperature is stirred at 150-200 DEG C
Mixing carries out condensation reaction, after reaction 30-60min, cools down at room temperature；
(4) crude product water dissolves, are subsequently adding 40% KOH solution regulation pH to 7.5-8.0, directly
Filtering, crystallisation by cooling are that can obtain finished product, high purity 92-95%, and steel ball is reclaimed after can be taken off cleaning
Recycle.
In the technique of the invention, product purity is taken out at random using HPLC sampling Detections, i.e. product
10 tests of sample are averaged and are calculated.
In the technique of the invention, the reaction temperature in step (3) is preferably 170-190 DEG C.
In the technique of the invention, the reaction time in step (3) is preferably 50min.
In the technique of the invention, the pH in step (4) is preferably 7.8.
Compared with prior art, add in reaction mass dicyandiamide and ammonium nitrate in technical scheme
Enter thin steel ball, by the collision of steel ball, grinding material in stirring reaction, it is achieved thereby that material more fills
Tap is touched and reacted, and have effectively achieved the mesh for promoting reaction forward to carry out and at utmost avoiding side reaction
, so cause product in impurity content it is few, product purity is improved.Additionally, reaction temperature, when
Between and pH the appropriately selected generation that material overreaction can be avoided to trigger other impurity, in another kind
The raising fully carried out with product purity of reaction has been ensured in degree.
Technical scheme is suitable by the introducing of the steel ball of reusable edible and technological parameter
Optimization so that guanidine nitrate is capable of the production in enormous quantities of high-purity, with extensive industrial value and market
Prospect.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, but these exemplary embodiments are simultaneously
It is non-that any type of any restriction is constituted to real protection scope of the invention.
Embodiment 1
(1) ammonium nitrate is crushed, crosses 70 mesh sieves, the ammonium nitrate fine powder for sifting out is standby；
(2) by 5kg ammonium nitrate fine powder and 2.5kg dicyandiamides, and it is thin to mix a diameter of 8mm thereto
Steel ball 25, is well mixed；
(3) divide 3 batches complete charging, be placed in reactor, controlling reaction temperature at 180 DEG C, stir into
Row condensation reaction, after reaction 50min, cools down at room temperature；
(4) crude product water dissolves, the KOH solution for being subsequently adding 40% adjusts pH to 7.8, direct mistake
Filter, crystallisation by cooling are that can obtain finished product, guanidine nitrate molar yield 91%, and HPLC purity is 95%, steel
The recyclable recycling of pearl.
Embodiment 2
(1) ammonium nitrate is crushed, crosses 70 mesh sieves, the ammonium nitrate fine powder for sifting out is standby；
(2) by 5kg ammonium nitrate fine powder and 2.5kg dicyandiamides with 2:1 is matched, and is mixed thereto
A diameter of thin steel balls 25 of 8mm, are well mixed；
(3) divide 3 batches complete charging, be placed in reactor, controlling reaction temperature at 190 DEG C, stir into
Row condensation reaction, after reaction 30min, cools down at room temperature；
(4) crude product water dissolves, the KOH solution for being subsequently adding 40% adjusts pH to 7.5, direct mistake
Filter, crystallisation by cooling are that can obtain finished product, guanidine nitrate molar yield 89%, and HPLC purity is 92%, steel
The recyclable recycling of pearl.
Embodiment 3
(1) ammonium nitrate is crushed, crosses 70 mesh sieves, the ammonium nitrate fine powder for sifting out is standby；
(2) by 10kg ammonium nitrate fine powder and 5kg dicyandiamides with 2:1 is matched, and is mixed thereto
A diameter of thin steel balls 50 of 8mm, are well mixed；
(3) divide 3 batches complete charging, be placed in reactor, controlling reaction temperature at 170 DEG C, stir into
Row condensation reaction, after reaction 60min, cools down at room temperature；
(4) crude product water dissolves, the KOH solution for being subsequently adding 40% adjusts pH to 8.0, direct mistake
Filter, crystallisation by cooling are that can obtain finished product, guanidine nitrate molar yield 88%, and HPLC purity is 93%, steel
The recyclable recycling of pearl.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit of the invention
Protection domain.Additionally, it will also be appreciated that after technology contents of the invention have been read, art technology
Personnel can make various changes, modification and/or modification to the present invention, and all these equivalent form of value equally falls
Within the protection domain that the application appended claims are limited.
Claims (5)
1. a kind of preparation technology of guanidine nitrate, its concrete technology step is as follows：
(1) ammonium nitrate is crushed, crosses 70 mesh sieves, the ammonium nitrate fine powder for sifting out is standby；
(2) by ammonium nitrate fine powder and dicyandiamide with 2:1 is matched, and mixes a diameter of 8mm thereto
Thin steel ball, is well mixed, wherein dicyandiamide quality:The number of steel ball is 100:1g/；
(3) divide 3 batches to complete charging, be placed in reactor, controlling reaction temperature is stirred at 150-200 DEG C
Mixing carries out condensation reaction, after reaction 30-60min, cools down at room temperature；
(4) crude product water dissolves, are subsequently adding 40% KOH solution regulation pH to 7.5-8.0, directly
Filtering, crystallisation by cooling are that can obtain finished product, the recyclable recycling of steel ball.
2. the preparation technology of guanidine nitrate as claimed in claim 1, it is characterised in that：The step (3)
In reaction temperature be preferably 170-190 DEG C.
3. the preparation technology of guanidine nitrate as claimed in claim 1 or 2, it is characterised in that：The step
Suddenly the reaction time in (3) be preferably 50min.
4. the preparation technology of the guanidine nitrate as described in claim any one of 1-3, it is characterised in that：Institute
The pH stated in step (4) is preferably 7.8.
5. the preparation technology of the guanidine nitrate as described in claim any one of 1-4, it is characterised in that：Produce
Product purity uses HPLC sampling Detections, i.e. 10 tests of product random sampling to average and be calculated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510852889.0A CN106810470A (en) | 2015-11-27 | 2015-11-27 | A kind of preparation technology of guanidine nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510852889.0A CN106810470A (en) | 2015-11-27 | 2015-11-27 | A kind of preparation technology of guanidine nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106810470A true CN106810470A (en) | 2017-06-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510852889.0A Pending CN106810470A (en) | 2015-11-27 | 2015-11-27 | A kind of preparation technology of guanidine nitrate |
Country Status (1)
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| CN (1) | CN106810470A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111087326A (en) * | 2020-01-13 | 2020-05-01 | 宁夏贝利特生物科技有限公司 | Method for refining guanidine nitrate |
-
2015
- 2015-11-27 CN CN201510852889.0A patent/CN106810470A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111087326A (en) * | 2020-01-13 | 2020-05-01 | 宁夏贝利特生物科技有限公司 | Method for refining guanidine nitrate |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170609 |
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| WD01 | Invention patent application deemed withdrawn after publication |