CN112707848A - Preparation method of guanidine hydrochloride - Google Patents
Preparation method of guanidine hydrochloride Download PDFInfo
- Publication number
- CN112707848A CN112707848A CN201911021935.7A CN201911021935A CN112707848A CN 112707848 A CN112707848 A CN 112707848A CN 201911021935 A CN201911021935 A CN 201911021935A CN 112707848 A CN112707848 A CN 112707848A
- Authority
- CN
- China
- Prior art keywords
- guanidine hydrochloride
- reaction
- preparation
- dissolving
- weight
- 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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Links
- 229960000789 guanidine hydrochloride Drugs 0.000 title claims abstract description 28
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 8
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 7
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007086 side reaction 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
-
- 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
- C07C277/06—Purification or separation of guanidine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of a chemical product, in particular to a preparation method of guanidine hydrochloride, which comprises the following steps: a. melting, b, dissolving, c, filtering, d, dehydrating, e, crystallizing and obtaining the finished guanidine hydrochloride product with the yield higher than 95%. The reaction process is simple, the steps of adding raw materials, heating a reaction kettle and subsequent purification are not repeated, the energy consumption is reduced, the reaction time is shortened, byproducts are greatly reduced, and the yield is improved.
Description
Technical Field
The invention relates to a preparation method of a chemical product, in particular to a preparation method of guanidine hydrochloride.
Background
In the existing production process of guanidine hydrochloride, dicyandiamide and ammonium salt (ammonium chloride) are generally used as raw materials, and are subjected to melt reaction at 170-230 ℃ to obtain a guanidine hydrochloride crude product, and the guanidine hydrochloride crude product is refined to obtain a finished product. In the refining process, raw materials need to be added repeatedly, the reaction kettle needs to be heated, and subsequent purification steps need to be carried out, so that the reaction energy consumption and the reaction time are greatly increased, and meanwhile, a large number of byproducts are generated and the yield is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, an improved preparation method of guanidine hydrochloride is provided.
The technical scheme adopted by the invention is as follows: a preparation method of guanidine hydrochloride comprises the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
In the melting step, after heating to 165 ℃, the heating is stopped, the reaction is carried out for 3 hours, and the temperature is increased from 165 ℃ to 185 ℃. The melting reaction temperature is up to 185 ℃, and side reaction is difficult to occur at the temperature, so that byproducts are greatly reduced, and the yield is improved.
In the dissolving step, alkali is added into the solution so as to treat the residual ammonium salt in the reaction.
Compared with the prior art, the invention has the following advantages: the reaction process is simple, the steps of adding raw materials, heating a reaction kettle and subsequent purification are not repeated, the energy consumption is reduced, the reaction time is reduced, the reaction temperature is up to 185 ℃, byproducts are greatly reduced, and the yield is improved.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the embodiments of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A preparation method of guanidine hydrochloride comprises the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
In the melting step, heating was stopped after heating to 165 ℃ and the reaction was stopped for 3 hours, and the temperature was raised from 165 ℃ to 185 ℃.
In the dissolving step, an alkali is added to the solution.
Claims (2)
1. The preparation method of guanidine hydrochloride is characterized by comprising the following steps:
a. melting: adding raw materials of dicyandiamide and ammonium chloride into a reaction kettle according to the weight ratio of 1: 1.27, adding a catalyst of zinc chloride, heating to 165 ℃, preserving heat for 3 hours, and carrying out a melting reaction to obtain a guanidine hydrochloride crude product;
b. dissolving: at normal temperature, dissolving the guanidine hydrochloride crude product in water according to the ratio of 1: 1;
c. and (3) filtering: removing raw materials, catalysts and reaction byproducts by a filtering method;
d. and (3) dehydrating: dehydrating the filtered mother liquor;
e. and (3) crystallization: cooling the supersaturated solution, concentrating and crystallizing to obtain a guanidine hydrochloride finished product;
wherein the input weight of the catalyst zinc chloride is 0.5 percent of the weight of the raw material dicyandiamide, and the weight percentage content of the guanidine hydrochloride in the finished product of the guanidine hydrochloride is more than 95 percent.
2. The method of preparing guanidine hydrochloride according to claim 1, wherein: in the dissolving step, alkali is added into the solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911021935.7A CN112707848A (en) | 2019-10-25 | 2019-10-25 | Preparation method of guanidine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911021935.7A CN112707848A (en) | 2019-10-25 | 2019-10-25 | Preparation method of guanidine hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112707848A true CN112707848A (en) | 2021-04-27 |
Family
ID=75540546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911021935.7A Pending CN112707848A (en) | 2019-10-25 | 2019-10-25 | Preparation method of guanidine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112707848A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113754567A (en) * | 2021-10-13 | 2021-12-07 | 宁夏蓝白黑循环科技有限公司 | Novel preparation process of refined guanidine carbonate |
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385419A (en) * | 2002-06-14 | 2002-12-18 | 方建文 | Process for preparing guanidine hydrochloride |
| CN102079725A (en) * | 2011-01-27 | 2011-06-01 | 台州市尔康药业有限公司 | Method for preparing 2-chloropyrimidine |
-
2019
- 2019-10-25 CN CN201911021935.7A patent/CN112707848A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385419A (en) * | 2002-06-14 | 2002-12-18 | 方建文 | Process for preparing guanidine hydrochloride |
| CN102079725A (en) * | 2011-01-27 | 2011-06-01 | 台州市尔康药业有限公司 | Method for preparing 2-chloropyrimidine |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113754567A (en) * | 2021-10-13 | 2021-12-07 | 宁夏蓝白黑循环科技有限公司 | Novel preparation process of refined guanidine carbonate |
| CN113754567B (en) * | 2021-10-13 | 2024-02-20 | 宁夏蓝白黑循环科技有限公司 | Preparation process of novel refined guanidine carbonate |
| 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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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210427 |
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| RJ01 | Rejection of invention patent application after publication |