CN109232324A - A kind of novel purification guanidine hydrochloride is synthetically prepared production technology - Google Patents
A kind of novel purification guanidine hydrochloride is synthetically prepared production technology Download PDFInfo
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- CN109232324A CN109232324A CN201811363064.2A CN201811363064A CN109232324A CN 109232324 A CN109232324 A CN 109232324A CN 201811363064 A CN201811363064 A CN 201811363064A CN 109232324 A CN109232324 A CN 109232324A
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- CN
- China
- Prior art keywords
- reaction kettle
- guanidine hydrochloride
- glass bar
- synthetically prepared
- production technology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229960000789 guanidine hydrochloride Drugs 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 238000005516 engineering process Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 239000011521 glass Substances 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 17
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 12
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 9
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 9
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 239000007787 solid Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of novel purification guanidine hydrochlorides to be synthetically prepared production technology, including being synthetically prepared raw material and tool: dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g, reaction kettle one, one, porcelain measuring cup, glass bar one, precise electronic balance one, beneficial effects of the present invention: for the present invention using no cutting edge of a knife or a sword glass bar, glass bar is that both ends diameter is identical and without curved glass bar, use the preceding drying for guaranteeing glass bar surface, it is relatively solid without cutting edge of a knife or a sword glass bar, prevent glass dregs fracture in whipping process, the consummate degree of the guanidine hydrochloride of the behind of guarantee；The measurement accuracy of precise electronic balance is every graduation indication 1g weight, keeps proportion process more accurate；Reaction kettle is equipped with temperature sensor, the convenient temperature environment monitored in reaction kettle at any time；Temperature sensor on reaction kettle is the KGW5 type temperature sensor with digital display panel, keeps temperature data more intuitive, facilitates observation.
Description
Technical field:
The invention belongs to guanidine hydrochloride fabricating technology field, it is related to a kind of novel purification guanidine hydrochloride and is synthetically prepared production work
Skill.
Background technique:
Traditional guanidine hydrochloride synthesis and preparation process of forbidding is simple proportion, and the operation in each process is not rigorous such as:
Impurity, temperature are mixed when stirring to be difficult to observe, match weighing inaccurately etc., will lead to the consummate degree of the guanidine hydrochloride after being synthetically prepared
Bottom is easy doping and reacts incomplete problem.
Summary of the invention:
The object of the invention is that providing a kind of novel purification guanidine hydrochloride to solve the above-mentioned problems is synthetically prepared life
Production. art solves the disadvantage that in the prior art.
To solve the above-mentioned problems, the present invention provides a kind of technical solutions:
A kind of novel purification guanidine hydrochloride is synthetically prepared production technology, including is synthetically prepared raw material and tool: dicyandiamide
350g, ammonium chloride 450g, ammonium carbonate 50g, reaction kettle one, one, porcelain measuring cup, glass bar one, precise electronic balance one
It is a.
Preferably, the reaction kettle is the reaction kettle that capacity is 1L and included electric heating function, it is the preparation of guanidine hydrochloride
Heating environment is provided.
Preferably, the inner wall of the porcelain measuring cup and bottom are pure white, the preceding high temperature after over cleaning is dried of operation
Disinfection treatment facilitates the mixability of observation raw material and ensure that the gnotobasis in guanidine hydrochloride preparation process.
Preferably, the glass bar is no cutting edge of a knife or a sword glass bar, the glass bar is that both ends diameter is identical and without curved glass
Glass stick, using the preceding drying for guaranteeing glass bar surface, no cutting edge of a knife or a sword glass bar is relatively solid, prevents glass dregs fracture in whipping process
In, the consummate degree of the guanidine hydrochloride of the behind of guarantee.
Preferably, the measurement accuracy of the precise electronic balance is every graduation indication 1g weight, make proportion process more
Accurately.
Preferably, the reaction kettle is equipped with temperature sensor, the convenient temperature environment monitored in reaction kettle at any time.
Preferably, the temperature sensor on the reaction kettle is the KGW5 type temperature sensor with digital display panel, make
Temperature data is more intuitive, facilitates observation.
Preferably, the following steps are included:
One, it matches, by dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g is with dicyandiamide 168g: ammonium chloride 203g: carbonic acid
The ratio of ammonium 19g is by two parts of precise electronic day share system, and a prefabricated, another is spare.
Two, prepare, will be prefabricated after raw material be added to reaction kettle, spare raw material is added in porcelain measuring cup, is passed through
Raw material in glass bar uniform stirring reaction kettle uniformly adds in porcelain measuring cup after mixing evenly by the raw material in reaction kettle
Raw material；
Three, it heats, reaction kettle is heated to 170 DEG C ± 5 DEG C, and monitor by temperature sensor；
Four, synthetic reaction reacts three hours in 170 DEG C ± 5 DEG C of reaction kettle environment；
Five, preparation is completed, and is opened reaction kettle and is obtained guanidine hydrochloride 385g.
Beneficial effects of the present invention: reaction kettle of the invention is the reaction kettle that capacity is 1L and included electric heating function, side
Just heating environment is provided for the preparation of guanidine hydrochloride；The inner wall of porcelain measuring cup and bottom are pure white, are dried in the air before operation through over cleaning
High-temperature disinfection treatment after dry facilitates the mixability of observation raw material and ensure that the gnotobasis in guanidine hydrochloride preparation process；Glass
Glass stick is no cutting edge of a knife or a sword glass bar, glass bar is that both ends diameter is identical and without curved glass bar, uses the preceding glass bar surface that guarantees
Dry, no cutting edge of a knife or a sword glass bar is relatively solid, prevents glass dregs fracture in whipping process, the guanidine hydrochloride of the behind of guarantee it is consummate
Degree；The measurement accuracy of precise electronic balance is every graduation indication 1g weight, keeps proportion process more accurate；Reaction kettle is equipped with temperature
Spend sensor, the convenient temperature environment monitored in reaction kettle at any time；Temperature sensor on reaction kettle is with digital display panel
KGW5 type temperature sensor, keeps temperature data more intuitive, facilitates observation.
Detailed description of the invention:
Detailed description will be given by the following detailed implementation and drawings by the present invention for ease of explanation,.
Fig. 1 is that novel purification guanidine hydrochloride is synthetically prepared production technological process.
Specific embodiment:
As shown in Figure 1, present embodiment uses following technical scheme: a kind of novel purification guanidine hydrochloride is synthetically prepared life
Production. art, including it is synthetically prepared raw material and tool: dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g, reaction kettle one, porcelain
One, quality cup, glass bar one, precise electronic balance one.
Wherein, reaction kettle is the reaction kettle that capacity is 1L and included electric heating function, provides heating for the preparation of guanidine hydrochloride
Environment.
Wherein, the inner wall of porcelain measuring cup and bottom are pure white, the preceding high-temperature disinfection treatment after over cleaning is dried of operation,
Facilitate the mixability of observation raw material and ensure that the gnotobasis in guanidine hydrochloride preparation process.
Wherein, glass bar is no cutting edge of a knife or a sword glass bar, and glass bar is that both ends diameter is identical and without curved glass bar, uses preceding guarantor
The drying on glass bar surface is demonstrate,proved, no cutting edge of a knife or a sword glass bar is relatively solid, and prevent glass dregs fracture in whipping process, the behind of guarantee
The consummate degree of guanidine hydrochloride.
Wherein, the measurement accuracy of precise electronic balance is every graduation indication 1g weight, keeps proportion process more accurate.
Wherein, reaction kettle is equipped with temperature sensor, the convenient temperature environment monitored in reaction kettle at any time.
Wherein, the temperature sensor on reaction kettle is the KGW5 type temperature sensor with digital display panel, makes temperature data
It is more intuitive, facilitate observation.
Wherein, comprising the following steps:
One, it matches, by dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g is with dicyandiamide 168g: ammonium chloride 203g: carbonic acid
The ratio of ammonium 19g is by two parts of precise electronic day share system, and a prefabricated, another is spare.
Two, prepare, will be prefabricated after raw material be added to reaction kettle, spare raw material is added in porcelain measuring cup, is passed through
Raw material in glass bar uniform stirring reaction kettle uniformly adds in porcelain measuring cup after mixing evenly by the raw material in reaction kettle
Raw material；
Three, it heats, reaction kettle is heated to 170 DEG C ± 5 DEG C, and monitor by temperature sensor；
Four, synthetic reaction reacts three hours in 170 DEG C ± 5 DEG C of reaction kettle environment；
Five, preparation is completed, and is opened reaction kettle and is obtained guanidine hydrochloride 385g.
The present invention is by the way that by dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g is with dicyandiamide 168g: ammonium chloride 203g: carbon
The ratio of sour ammonium 19g is by two parts of precise electronic day share system, and a prefabricated, another is spare, will be prefabricated after raw material addition
To reaction kettle, spare raw material is added in porcelain measuring cup, by the raw material in glass bar uniform stirring reaction kettle, will be anti-
It answers the raw material in kettle uniformly to add the raw material in porcelain measuring cup after mixing evenly, reaction kettle is heated to 170 DEG C ± 5 DEG C, and lead to
The monitoring of excess temperature sensor, reacts three hours in 170 DEG C ± 5 DEG C of reaction kettle environment, opens reaction kettle and obtains guanidine hydrochloride
385g, wherein reaction kettle is the reaction kettle that capacity is 1L and included electric heating function, convenient to provide heating for the preparation of guanidine hydrochloride
Environment；The inner wall of porcelain measuring cup and bottom are pure white, and the preceding high-temperature disinfection treatment after over cleaning is dried of operation facilitates observation
The mixability of raw material simultaneously ensure that the gnotobasis in guanidine hydrochloride preparation process；Glass bar is no cutting edge of a knife or a sword glass bar, and glass bar is
Both ends diameter is identical and without curved glass bar, and using the preceding drying for guaranteeing glass bar surface, no cutting edge of a knife or a sword glass bar is relatively solid, prevents
Only glass dregs fracture is in whipping process, the consummate degree of the guanidine hydrochloride of the behind of guarantee；The measurement accuracy of precise electronic balance is
Every graduation indication 1g weight, keeps proportion process more accurate；Reaction kettle is equipped with temperature sensor, convenient to monitor reaction kettle at any time
Interior temperature environment；Temperature sensor on reaction kettle is the KGW5 type temperature sensor with digital display panel, makes temperature data
It is more intuitive, facilitate observation.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, the technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention, the claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of novel purification guanidine hydrochloride is synthetically prepared production technology, which is characterized in that including being synthetically prepared raw material and tool:
Dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g, reaction kettle one, one, porcelain measuring cup, glass bar one, precise electronic day
It is one flat.
2. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: described anti-
Answering kettle is the reaction kettle that capacity is 1L and included electric heating function.
3. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: the porcelain
The inner wall of quality cup and bottom are pure white, the preceding high-temperature disinfection treatment after over cleaning is dried of operation.
4. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: the glass
Glass stick is no cutting edge of a knife or a sword glass bar, and the glass bar is that both ends diameter is identical and without curved glass bar, uses preceding guarantee glass bar table
The drying in face.
5. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: the electricity
The measurement accuracy of sub- precision balance is every graduation indication 1g weight.
6. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: described anti-
Kettle is answered to be equipped with temperature sensor.
7. a kind of novel purification guanidine hydrochloride according to claim 6 is synthetically prepared production technology, it is characterised in that: described anti-
Answering the temperature sensor on kettle is the KGW5 type temperature sensor with digital display panel.
8. a kind of novel purification guanidine hydrochloride according to claim 1 is synthetically prepared production technology, it is characterised in that: including with
Lower step:
One, it matches, by dicyandiamide 350g, ammonium chloride 450g, ammonium carbonate 50g is with dicyandiamide 168g: ammonium chloride 203g: ammonium carbonate
The ratio of 19g is by two parts of precise electronic day share system, and a prefabricated, another is spare.
Two, prepare, will be prefabricated after raw material be added to reaction kettle, spare raw material is added in porcelain measuring cup, glass is passed through
Raw material in reaction kettle is uniformly being added the original in porcelain measuring cup by the raw material in stick uniform stirring reaction kettle after mixing evenly
Material；
Three, it heats, reaction kettle is heated to 170 DEG C ± 5 DEG C, and monitor by temperature sensor；
Four, synthetic reaction reacts three hours in 170 DEG C ± 5 DEG C of reaction kettle environment；
Five, preparation is completed, and is opened reaction kettle and is obtained guanidine hydrochloride 385g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811363064.2A CN109232324A (en) | 2018-11-15 | 2018-11-15 | A kind of novel purification guanidine hydrochloride is synthetically prepared production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811363064.2A CN109232324A (en) | 2018-11-15 | 2018-11-15 | A kind of novel purification guanidine hydrochloride is synthetically prepared production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109232324A true CN109232324A (en) | 2019-01-18 |
Family
ID=65074862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811363064.2A Pending CN109232324A (en) | 2018-11-15 | 2018-11-15 | A kind of novel purification guanidine hydrochloride is synthetically prepared production technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302977A (en) * | 2020-03-18 | 2020-06-19 | 湖南吴赣药业有限公司 | Purification method of pharmaceutical grade guanidine hydrochloride |
| CN115286538A (en) * | 2022-07-12 | 2022-11-04 | 烟台三鼎化工有限公司 | Antibacterial guanidine hydrochloride efficient crystallization drying process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50129521A (en) * | 1974-03-25 | 1975-10-13 | ||
| CN1385419A (en) * | 2002-06-14 | 2002-12-18 | 方建文 | Process for preparing guanidine hydrochloride |
| CN103951591A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine hydrochloride |
-
2018
- 2018-11-15 CN CN201811363064.2A patent/CN109232324A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50129521A (en) * | 1974-03-25 | 1975-10-13 | ||
| CN1385419A (en) * | 2002-06-14 | 2002-12-18 | 方建文 | Process for preparing guanidine hydrochloride |
| CN1247536C (en) * | 2002-06-14 | 2006-03-29 | 方建文 | Process for preparing guanidine hydrochloride |
| CN103951591A (en) * | 2014-05-19 | 2014-07-30 | 宁夏贝利特化工有限公司 | Production technique of guanidine hydrochloride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302977A (en) * | 2020-03-18 | 2020-06-19 | 湖南吴赣药业有限公司 | Purification method of pharmaceutical grade guanidine hydrochloride |
| CN111302977B (en) * | 2020-03-18 | 2022-05-17 | 湖南吴赣药业有限公司 | Purification method of pharmaceutical grade guanidine hydrochloride |
| CN115286538A (en) * | 2022-07-12 | 2022-11-04 | 烟台三鼎化工有限公司 | Antibacterial guanidine hydrochloride efficient crystallization drying process |
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| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 753000 Taisha Road, Taisha Industrial Park, Pingluo County, Shizuishan City, Ningxia Hui Autonomous Region Applicant after: Ningxia blue white black Recycling Technology Co.,Ltd. Address before: 753000 Taisha Road, Taisha Industrial Park, Pingluo County, Shizuishan City, Ningxia Hui Autonomous Region Applicant before: NINGXIA NINGHANG CYCLE TECHNOLOGY Co.,Ltd. |
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Application publication date: 20190118 |